CN106903324A - A kind of preparation method of Graphene-nano silver dispersion - Google Patents
A kind of preparation method of Graphene-nano silver dispersion Download PDFInfo
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- CN106903324A CN106903324A CN201510970957.3A CN201510970957A CN106903324A CN 106903324 A CN106903324 A CN 106903324A CN 201510970957 A CN201510970957 A CN 201510970957A CN 106903324 A CN106903324 A CN 106903324A
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- graphene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention belongs to nano material field of functional materials, a kind of preparation method of graphene nano silver dispersion liquid is refered in particular to, its preparation method is：（1）Liquid phase method prepares graphene suspension；（2）The separation and purification of graphene dispersing solution；（3）The preparation of graphene nano silver crystal seed liquid；（4）Electronation prepares graphene nano silver dispersion liquid.The advantage of the invention is that using the skin effect of nano material, suction-operated causes that nano-Ag particles are preferentially adsorbed on graphene film layer surface, so as to prepare good electric conductivity, and the graphene nano silver dispersion liquid of good dispersion, and the method program is simple, easily operated, product efficiency is high.
Description
Technical field
The invention belongs to inorganic functional material technical field, and in particular to a kind of preparation of Graphene-nano silver dispersion
Method.
Background technology
Argent has excellent physicochemical characteristics, such as optimal normal temperature electric conductivity, thermal conductivity, most cheap high temperature resistance
The noble metal of oxidation, most strong reflection characteristic, photosensitive imaging characteristic, and anti-inflammation characteristic, make it be widely used in modern work
Industry field.Because the particle diameter of nano-silver powder is small, active height, special chemical that Nano Silver is shown and physical, and its in light
The potential using value in the fields such as electronics, SERS base materials, optical tag, near-field optical probe makes it receive much concern, with electronics
Light, small, the thin trend for electrically continuing to develop, makes nano-silver powder turn into one of main application direction in microelectronics industry.
Graphene (Graphene) is the Two-dimensional Carbon atomic crystal of monoatomic thickness, the resistance that electronics is transmitted in Graphene
Power very little, is the ideal material of nanometric circuit with good electronic transport property.At present, on Graphene and nano-particle
Compound report also has many, such as Publication No. CN102515560 Chinese invention patents《One kind prepares Graphene/Ag composite guides
Conductive film》, the method that one kind prepares Graphene/Ag composite conductive thin films is disclosed, with graphene oxide/silver sol as preceding
Drive body, using czochralski method, heat treatment after obtain transparent conductive film.The and for example patent of invention of Publication No. CN102136306A
Application, it is disclosed《Ag/ graphene nanometer conductive compound materials and preparation method thereof》Prepared there is provided an a kind of stage reduction method
The method of silver/graphite alkene composite.But, these reports is limited to the composite of graphene oxide and nano-particle, by
Substantial amounts of oxygen-containing group functional group is introduced in the surface and edge of graphene oxide, for the attachment of nano-particle provides position,
Graphene oxide is also allowed for be stably dispersed in some polar solvents.But graphene oxide loses it due to the presence of oxygen-containing group
Good conductive capability has been lost, and this defect is difficult to repair, therefore the electrical property of the composite of the method preparation is difficult
Meet and require, and be then unfavorable for the absorption and dispersion of nano-particle using pure Graphene.A kind of Graphene of present invention offer-receive
The preparation method of the silver-colored suspension of rice, chemistry is passed through after preparing Graphene, and centrifugation by liquid phase method in Graphene solvent
Reduction method for preparing nanometer silver, obtains Graphene-nano silver dispersion well dispersed and with excellent conductive capability.
The content of the invention
For the defect of graphene oxide, it is an object of the invention to provide a kind of system of Graphene-nano silver suspending liquid
Preparation Method, nanometer is prepared after preparing Graphene, and centrifugation by liquid phase method in Graphene solvent by chemical reduction method
Silver, obtains well dispersed Graphene-nano silver suspending liquid.
Preparation technology is：
（1）Liquid phase method prepares graphene suspension：By in appropriate graphite powder and dispersant addition solvent, 90 ~ 110 DEG C are heated to
Ultrasound peels off 0.5 ~ 2h；
（2）The separation and purification of graphene dispersing solution：The centrifugation under 4000r/min rotating speeds, takes upper liquid stand-by after separation；
（3）The preparation of Graphene-Nano Silver crystal seed liquid：It is configured to the certain silver nitrate of concentration ratio, polyvinylpyrrolidone（PVP）
The aqueous solution, a certain proportion of graphene solution is sufficiently mixed with above silver nitrate solution, is placed in power in the micro- of 100 ~ 400W
1 ~ 10min is reduced in ripple reactor, is crystal seed liquid.
（4）The preparation of Graphene-nano silver dispersion：PH is adjusted after Graphene-Nano Silver crystal seed liquid is stirred, after
0.5 ~ 1h of continuous ultrasonic agitation；To 40 ~ 80 DEG C, it is to obtain Graphene-nanometer to add 1.5 ~ 2h of reducing agent ultrasonic agitation to regulation temperature
Silver-colored dispersion liquid.
Step（1）Described dispersant is selected from neopelex（SDBS）, polyvinylpyrrolidone（PVP）, ox
Yellow NaTDC（STC）, lauryl dimethyl amine bromide（CTAB）, one or more in trisodium citrate.
Step（1）Described solvent is selected from deionized water, dimethyl sulfoxide (DMSO)（DMSO）, N-methyl pyrrolidones（NMP）, two
NMF（DMF）, tetrahydrofuran（THF）In one or more.
Graphite powder concentration in a solvent is 0.01 ~ 5mg/ml.
Step（1）Dispersant concentration in a solvent is 0.01 ~ 0.5g/ml.
Step（3）The concentration of the silver nitrate is 0.01 ~ 0.1g/ml, and PVP is 1 ~ 5 with the mass ratio of silver nitrate.
Step（3）Silver nitrate is water-soluble and step（2）The volume ratio of solvent is 0.2 ~ 2.
Step（4）Described reducing agent is selected from sodium borohydride, hydrazine hydrate, ascorbic acid, glucose, formaldehyde
One or more.
The advantage of the invention is that being prepared for the excellent graphene dispersing solution of structural integrity, electric conductivity using liquid phase method；
Choose can the solvent of effectively dispersed graphite alkene mix with deionized water, prepare silver nitrate/graphene dispersing solution, and utilization PVP
Reproducibility is prepared for Nano Silver crystal seed liquid under microwave condition.There is the specific surface of superelevation using Nano Silver crystal seed in reduction process
Can be acted on the adsorption of Graphene, made by Nano Silver crystal seed Preferential adsorption in graphenic surface.Further added after reduction
Appropriate dispersant obtains the Graphene-nano silver dispersion of good dispersion and electric conductivity.
Specific embodiment
Embodiment 1
It is 1 by mass ratio:1 graphite powder is configured to 0.01mg/ml in mixing addition DMF with STC（Graphite powder）Mixture, rise
Temperature is to 100 DEG C of ultrasound 1h in the ultrasonic container of 400W power.The solution is taken after cooling to be centrifuged under conditions of 4000r/min
60min, takes upper liquid for graphene dispersing solution.It is 1 by mass ratio:1 silver nitrate is prepared in mixing addition deionized water with PVP
Into 0.05mg/ml（AgNO3）Solution, by volume 1:1 mixes silver nitrate solution and graphene dispersing solution, after stirring
It is placed in and 5min is reacted in the microwave reactor of 300W power, is added dropwise 0.1g/ml's under the stir speed (S.S.) of 100r/min after taking-up
Sodium hydroxide solution adjusts PH to 10, ultrasonic agitation 30min；60 DEG C are warming up to, body is slowly added dropwise under conditions of ultrasonic agitation
Product is than being 1:10 concentration is the glucose solution of 1g/ml；Constant temperature 1.5h terminates reaction.Obtain finely dispersed Graphene-receive
, be coated onto solution rod on glass baseplate after washing part dispersant by the silver-colored solution of rice, and 150 DEG C of roasting 30min, conductivity is small
In 1.0 × 10-5Ω•cm。
Embodiment 2
It is 1 by mass ratio:1 graphite powder is configured to 0.1mg/ml in mixing addition DMF with STC（Graphite powder）Mixture, rise
Temperature is to 100 DEG C of ultrasound 1h in the ultrasonic container of 400W power.The solution is taken after cooling to be centrifuged under conditions of 4000r/min
60min, takes upper liquid for graphene dispersing solution.It is 1 by mass ratio:2 silver nitrate is prepared in mixing addition deionized water with PVP
Into 0.05mg/ml（AgNO3）Solution, by volume 2:3 mix silver nitrate solution and graphene dispersing solution, after stirring
It is placed in and 5min is reacted in the microwave reactor of 300W power, is added dropwise 0.1g/ml's under the stir speed (S.S.) of 100r/min after taking-up
Sodium hydroxide solution adjusts PH to 10, ultrasonic agitation 30min；60 DEG C are warming up to, body is slowly added dropwise under conditions of ultrasonic agitation
Product is than being 1:10 concentration is the glucose solution of 1g/ml；Constant temperature 1.5h terminates reaction.Obtain finely dispersed Graphene-receive
, be coated onto solution rod on glass baseplate after washing part dispersant by the silver-colored solution of rice, and 150 DEG C of roasting 30min, conductivity is small
In 1.0 × 10-5Ω•cm。
Claims (8)
1. a kind of preparation method of Graphene-nano silver dispersion, it is characterized in that：Comprise the following steps：
（1）Liquid phase method prepares graphene suspension：By in appropriate graphite powder and dispersant addition solvent, 90 ~ 110 DEG C are heated to
Ultrasound peels off 0.5 ~ 2h；
（2）The separation and purification of graphene dispersing solution：The centrifugation under 4000r/min rotating speeds, takes upper liquid stand-by after separation；
（3）The preparation of Graphene-Nano Silver crystal seed liquid：It is configured to the certain silver nitrate of concentration ratio, polyvinylpyrrolidone（PVP）
The aqueous solution, a certain proportion of graphene solution is sufficiently mixed with above silver nitrate solution, is placed in power in the micro- of 100 ~ 400W
1 ~ 10min is reduced in ripple reactor, is crystal seed liquid；
（4）The preparation of Graphene-nano silver dispersion：PH is adjusted after Graphene-Nano Silver crystal seed liquid is stirred, continues super
Sound stirs 0.5 ~ 1h；To 40 ~ 80 DEG C, it is to obtain Graphene-Nano Silver point to add 1.5 ~ 2h of reducing agent ultrasonic agitation to regulation temperature
Dispersion liquid.
2. a kind of preparation method of Graphene-nano silver dispersion according to claim 1, it is characterized in that：Step（1）It is described
Dispersant be selected from neopelex（SDBS）, polyvinylpyrrolidone（PVP）, cow-bezoar NaTDC（STC）, ten
Dialkyl dimethyl amine bromide（CTAB）, one or more in trisodium citrate.
3. a kind of preparation method of Graphene-nano silver dispersion according to claim 1, it is characterized in that：Step（1）It is described
Solvent be selected from deionized water, dimethyl sulfoxide (DMSO)（DMSO）, N-methyl pyrrolidones（NMP）, dimethylformamide（DMF）, four
Hydrogen furans（THF）In one or more.
4. a kind of preparation method of Graphene-nano silver dispersion according to claim 1, it is characterized in that：Step（1）It is described
Graphite powder concentration in a solvent is 0.01 ~ 5mg/ml.
5. a kind of preparation method of Graphene-nano silver dispersion according to claim 1, it is characterized in that：Step（1）It is described
Dispersant concentration in a solvent is 0.01 ~ 0.5g/ml.
6. a kind of preparation method of Graphene-nano silver dispersion according to claim 1, it is characterized in that：Step（3）It is described
The concentration of silver nitrate is 0.01 ~ 0.1g/ml, and PVP is 1 ~ 5 with the mass ratio of silver nitrate.
7. a kind of preparation method of Graphene-nano silver dispersion according to claim 1, it is characterized in that：Step（3）Nitric acid
Silver-colored water-soluble and step（2）The volume ratio of solvent is 0.2 ~ 2.
8. a kind of preparation method of Graphene-nano silver dispersion according to claim 1, it is characterized in that：Step（4）It is described
Reducing agent be selected from sodium borohydride, hydrazine hydrate, ascorbic acid, glucose, formaldehyde in one or more.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108115151A (en) * | 2017-12-25 | 2018-06-05 | 哈尔滨工业大学 | A kind of in-situ reduction preparation method of the redox graphene hybrid structure of nanometer of modified by silver |
| CN108890170A (en) * | 2018-08-30 | 2018-11-27 | 桂林电子科技大学 | A kind of graphene-nano mattisolda Heat Conduction Material and preparation method thereof |
| CN109095942A (en) * | 2018-11-09 | 2018-12-28 | 张宏汉 | A kind of preparation method of building brick |
| CN109368629A (en) * | 2018-12-03 | 2019-02-22 | 广东电网有限责任公司 | A kind of graphene dispersion system and preparation method thereof |
| CN110089524A (en) * | 2018-01-31 | 2019-08-06 | 皇杰新能源科技(上海)有限公司 | Graphene coated nano silver antibacterial material and preparation method thereof |
| CN111099583A (en) * | 2018-10-26 | 2020-05-05 | 南京化学工业园环保产业协同创新有限公司 | Efficient composite synthesis method of graphene and nano-silver |
| CN111205513A (en) * | 2020-03-16 | 2020-05-29 | 厦门捌斗新材料科技有限公司 | Graphene-based heat-conducting composite filler and preparation method and application thereof |
| CN111292871A (en) * | 2019-12-27 | 2020-06-16 | 长沙新材料产业研究院有限公司 | Graphene-nano silver material and preparation method thereof |
| CN111715889A (en) * | 2020-06-22 | 2020-09-29 | 大连理工大学 | Method for preparing defect-free graphene/silver nanoparticle composite material by one-step method and application of defect-free graphene/silver nanoparticle composite material |
| CN112608642A (en) * | 2020-12-28 | 2021-04-06 | 长沙新材料产业研究院有限公司 | Ink-jet printing type graphene-doped nano-silver conductive ink and preparation method thereof |
| CN112993084A (en) * | 2021-02-04 | 2021-06-18 | 合肥工业大学 | Preparation method of Ag-rGO film with excellent photoelectric property |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108115151A (en) * | 2017-12-25 | 2018-06-05 | 哈尔滨工业大学 | A kind of in-situ reduction preparation method of the redox graphene hybrid structure of nanometer of modified by silver |
| CN110089524A (en) * | 2018-01-31 | 2019-08-06 | 皇杰新能源科技(上海)有限公司 | Graphene coated nano silver antibacterial material and preparation method thereof |
| CN108890170A (en) * | 2018-08-30 | 2018-11-27 | 桂林电子科技大学 | A kind of graphene-nano mattisolda Heat Conduction Material and preparation method thereof |
| CN111099583B (en) * | 2018-10-26 | 2022-04-29 | 南京化学工业园环保产业协同创新有限公司 | Efficient composite synthesis method of graphene and nano-silver |
| CN111099583A (en) * | 2018-10-26 | 2020-05-05 | 南京化学工业园环保产业协同创新有限公司 | Efficient composite synthesis method of graphene and nano-silver |
| CN109095942A (en) * | 2018-11-09 | 2018-12-28 | 张宏汉 | A kind of preparation method of building brick |
| CN109368629A (en) * | 2018-12-03 | 2019-02-22 | 广东电网有限责任公司 | A kind of graphene dispersion system and preparation method thereof |
| CN111292871A (en) * | 2019-12-27 | 2020-06-16 | 长沙新材料产业研究院有限公司 | Graphene-nano silver material and preparation method thereof |
| CN111205513A (en) * | 2020-03-16 | 2020-05-29 | 厦门捌斗新材料科技有限公司 | Graphene-based heat-conducting composite filler and preparation method and application thereof |
| CN111205513B (en) * | 2020-03-16 | 2021-08-31 | 厦门捌斗新材料科技有限公司 | Graphene-based heat-conducting composite filler and preparation method and application thereof |
| CN111715889B (en) * | 2020-06-22 | 2021-08-10 | 大连理工大学 | Method for preparing defect-free graphene/silver nanoparticle composite material by one-step method and application of defect-free graphene/silver nanoparticle composite material |
| CN111715889A (en) * | 2020-06-22 | 2020-09-29 | 大连理工大学 | Method for preparing defect-free graphene/silver nanoparticle composite material by one-step method and application of defect-free graphene/silver nanoparticle composite material |
| CN112608642A (en) * | 2020-12-28 | 2021-04-06 | 长沙新材料产业研究院有限公司 | Ink-jet printing type graphene-doped nano-silver conductive ink and preparation method thereof |
| CN112993084A (en) * | 2021-02-04 | 2021-06-18 | 合肥工业大学 | Preparation method of Ag-rGO film with excellent photoelectric property |
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