CN107159884A - Improve covering material of commercial graphites alkene microplate surface conductance performance and preparation method thereof - Google Patents

Improve covering material of commercial graphites alkene microplate surface conductance performance and preparation method thereof Download PDF

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CN107159884A
CN107159884A CN201710511013.9A CN201710511013A CN107159884A CN 107159884 A CN107159884 A CN 107159884A CN 201710511013 A CN201710511013 A CN 201710511013A CN 107159884 A CN107159884 A CN 107159884A
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covering material
nano
graphites alkene
commercial graphites
solution
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CN107159884B (en
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王源
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Nanjing Kai Yu Security Technology Co Ltd
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Nanjing Kai Yu Security Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0551Flake form nanoparticles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/068Flake-like particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/0666Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
    • C08G73/0672Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
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  • Polymers & Plastics (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Medicinal Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of covering material for improving commercial graphites alkene microplate surface conductance performance and preparation method thereof, on its composition, it is made up of commercial graphites alkene microplate and nano-Ag particles;In its size, nano-Ag particles particle diameter is between 50 200 nm;In its content, the mass ratio of commercial graphites alkene microplate and silver nano-grain is 4:1.7‑1:1.7 between;On its pattern, nano-Ag particles are grown in commercial graphites alkene microplate surface.The present invention is added in commercial graphites alkene slurry after a certain amount of material, and the graphene film layer electrical conductivity order of magnitude of preparation is from 101‑103S/m can be promoted to 103‑105S/m;Silver ion is adsorbed using the dopamine for being attached to commercial graphites alkene surface, reduction process is just for silver ion, and graphene does not produce the change of physicochemical property in the reaction, and experiment controllability is strong.

Description

Improve covering material of commercial graphites alkene microplate surface conductance performance and preparation method thereof
Technical field
It is more particularly to a kind of to improve commercial graphites alkene microplate surface conductance performance the invention belongs to field of nano material preparation Covering material and preparation method thereof.
Background technology
At present, China can the graphene of initial industrial metaplasia production institute is mainly prepared by oxidation-reduction method and liquid phase stripping method , with the characteristics of yield is high, method is easy, dispersive property is good in a solvent.However, being peeled off by oxidation-reduction method or liquid phase Graphene microchip prepared by method is stacked in the commercial graphites alkene film layer of composition, it is microcosmic present on multi-slice can cause between microplate Contact resistance increase, the small presence that can cause lattice defect in low conductive region area increase, monolithic in film layer of microplate size makes The electrical conductivity per piece of graphite alkene is obtained to decline.Above-mentioned three aspect factor, ultimately results in film layer whole conductivity actual value and (is less than 104S/m) with theoretical value (108S/m) differ greatly.Therefore, in commercial graphites alkene Surface coating high conductive material, reduction piece and piece Contact resistance between surface, improves lattice defect in monolithic, is the important technical for improving graphene film layer electric conductivity.
The content of the invention
It is an object of the invention to provide a kind of covering material for improving commercial graphites alkene microplate surface conductance performance and its preparation Method.
Realizing the object of the invention technical solution is:
It is micro- by commercial graphites alkene on a kind of covering material for improving commercial graphites alkene microplate surface conductance performance, its composition Piece and nano-Ag particles composition;In its size, nano-Ag particles particle diameter is between 50-200nm;In its content, commercial graphites alkene The mass ratio of microplate and silver nano-grain is 4:1.7-1:1.7 between;On its pattern, nano-Ag particles are grown in commercial graphites Alkene microplate surface.
A kind of preparation method for the covering material for improving above-mentioned commercial graphites alkene surface conductance performance, its step is as follows:
Step 1:Commercial graphites alkene is scattered in Tris aqueous slkalis of the concentration between 1-2mg/mL, concentration is made in 3- Dispersion liquid between 10mg/mL;
Step 2:Dopamine hydrochloride is added in dispersion liquid into step 1 so that Dopamine hydrochloride is dense in dispersion liquid Degree is between 0.5-1.5mg/mL;
Step 3:Dispersion liquid made from step 2 is at the uniform velocity stirred and filtered after more than 24 hours, the washing of gained solid matter, vacuum Dry;
Step 4:Ammoniacal liquor is instilled into 0.05-0.2mol/L silver nitrate solution to solution clear, by every liter of preparation Silver nitrate solution in add obtained solid matter in 20g steps 3, resulting solution is uniformly dispersed;
Step 5:Formaldehyde-alcohol-water mixed solution is prepared, the wherein volume ratio between formaldehyde, ethanol, water is 1:4:20;
Step 6:The solution that step 5 is prepared by volume 2:1 is added in step 4 resulting solution, persistently stirs 2 small When more than, solution after reaction is filtered, after deposit is cleaned through deionized water and ethanol, vacuum drying obtains described Covering material.
Compared with prior art, it is an advantage of the invention that:
(1) it is an advantage of the current invention that being added in commercial graphites alkene slurry after a certain amount of material, the stone of preparation The black alkene film layer electrical conductivity order of magnitude is from 101-103S/m can be promoted to 103-105S/m。
(2) it is an advantage of the current invention that adsorbing silver ion using the dopamine for being attached to commercial graphites alkene surface, reduced Journey is just for silver ion, and graphene does not produce the change of physicochemical property in the reaction, and experiment controllability is strong.
Brief description of the drawings
Fig. 1 is the preparation flow figure of covering material of the present invention.
Fig. 2 is the scanning electron microscope image of covering material of the present invention.
Embodiment
Idea of the invention is that:The oxygen-containing functional group on commercial graphites alkene surface is almost removed completely, surface chemistry inertia It is relatively strong, it polymerize to form layer of surface there is the poly- of amino structure in carbon nano tube surface using nontoxic, efficient Dopamine hydrochloride Layer is closed, silver ion is adsorbed onto commercial graphites alkene surface by the way that these amino structures are effective, then by silver ion reduction is nanometer Argent grain obtains the material.The preparation flow figure of material of the present invention is as shown in Figure 1.
Embodiment 1:
From commercially available commercial graphites alkene, experimental procedure is as follows:
Step 1:Commercial graphites alkene is dispersed in Tris aqueous slkalis, and wherein commercial graphites alkene concentration is 3mg/mL, Tris alkali Concentration is 1mg/mL.
Step 2:Dopamine hydrochloride is added in dispersion liquid into step 1, concentration is 0.5mg/mL.
Step 3:Dispersion liquid made from step 2 is at the uniform velocity stirred and filtered after more than 24 hours, gained solid matter is washed, very Sky is dried;
Step 4:0.05mol/L silver nitrate aqueous solution is prepared, ammoniacal liquor is instilled into the solution to solution clear, is pressed The solid matter obtained in 20g steps 3 is added in the silver nitrate aqueous solution of every liter of preparation, gained is uniformly dispersed.
Step 5:Formaldehyde-alcohol-water mixed solution is prepared, the wherein volume ratio between formaldehyde, ethanol and water is 1:4:20.
Step 6:The solution that step 5 is prepared is poured into step 4 resulting solution, step 4 and the volume ratio of step 5 solution For 2:1, persistently stir more than 2 hours, solution after reaction is filtered, after deposit is cleaned through deionized water and ethanol, Vacuum drying, is improved the covering material of commercial graphites alkene microplate surface conductance performance.
The microscopic appearance that the covering material is made is as shown in Figure 2.
The particle diameter of nano-Ag particles in the covering material is made at 50-200 nanometers.
The mass ratio that commercial graphites alkene and nano-Ag particles in the covering material are made is 4:1.7.
The covering material is added in commercial graphites alkene/aqueous dispersions that mass fraction is 5%, the nano material The 10% of the net quality of graphene is accounted for, film layer is made, film layer preparation method is as follows:
Step a:Compound concentration is 0.1g/L Tris aqueous slkalis, and the nano material is scattered in the solution by 10g/L;
Step b:Dopamine hydrochloride is added in dispersion liquid into step a so that the concentration of Dopamine hydrochloride in the solution For 0.1g/L;
Step c:Dispersion liquid is at the uniform velocity stirred and filtered after 24 hours, and solid matter spends deionized water and ethanol cyclic washing, Vacuum oven;
Step d:The nano material after step c aforementioned processings is added in graphene slurries, is uniformly mixed, Wherein described nano material accounts for the 10% of the net quality of graphene.
Electrical conductivity it is as shown in table 1.Commercial graphites alkene film layer electrical conductivity is promoted to 17992S/m from 8000S/m.
The electrical conductivity of 1 embodiment of table 1
Electrical conductivity (S/m)
The commercial graphites alkene film layer of embodiment 1 is not added 8000
Add the commercial graphites alkene film layer of embodiment 1 17992
Embodiment 2
Experimental procedure is same as Example 1, and wherein Tris alkaline concentrations are 2mg/mL, commercial graphites alkene dispersion liquid concentration For 10mg/mL, Dopamine hydrochloride concentration is 1.5mg/mL, and silver nitrate concentration is 0.2mol/L.
The particle diameter of nano-Ag particles in the covering material is made in 50-200nm.
The mass ratio that commercial graphites alkene and nano-Ag particles in the covering material are made is 1:1.7.
The covering material is added in commercial graphites alkene/aqueous dispersions that mass fraction is 5% and (purchased from Suzhou lattice Rui Feng), the nano material accounts for the 30% of the net quality of graphene, and the electrical conductivity that film layer is made is as shown in table 2.Commercial graphites alkene film Layer electrical conductivity is promoted to 97527S/m from 8000S/m.
The electrical conductivity of 1 embodiment of table 1
Electrical conductivity (S/m)
The commercial graphites alkene film layer of embodiment 2 is not added 8000
Add the commercial graphites alkene film layer of embodiment 2 97527
Embodiment 3
Experimental procedure is same as Example 1, and wherein Tris alkaline concentrations are 2mg/mL, commercial graphites alkene dispersion liquid concentration For 5mg/mL, Dopamine hydrochloride concentration is 1mg/mL, and silver nitrate concentration is 0.15mol/L.
The particle diameter of nano-Ag particles is in 50-200nm in the nano material prepared.
The mass ratio of commercial graphites alkene and nano-Ag particles is 1 in the nano material prepared:1.275.
The nano material is added in commercial graphites alkene/aqueous dispersions that mass fraction is 5% and (purchased from Suzhou lattice Rui Feng), the nano material accounts for the 50% of the net quality of graphene, and the electrical conductivity that film layer is made is as shown in table 2.Commercial graphites alkene film Layer electrical conductivity is promoted to 237590S/m from 8000S/m.
The electrical conductivity of 3 embodiment of table 3

Claims (7)

1. a kind of covering material for improving commercial graphites alkene microplate surface conductance performance, it is characterised in that on its composition, by industry Graphene microchip and nano-Ag particles composition;In its size, nano-Ag particles particle diameter is between 50-200 nm;In its content, work The mass ratio of industry graphene microchip and silver nano-grain is 4:1.7-1:1.7 between;On its pattern, nano-Ag particles are grown in Commercial graphites alkene microplate surface.
2. covering material as claimed in claim 1, it is characterised in that its preparation process is as follows:
Step 1:Commercial graphites alkene is scattered in Tris aqueous slkalis, dispersion liquid is made;
Step 2:Dopamine hydrochloride is added in dispersion liquid into step 1 so that concentration of the Dopamine hydrochloride in dispersion liquid exists Between 0.5-1.5 mg/mL;
Step 3:Dispersion liquid made from step 2 is at the uniform velocity stirred, filtered, the washing of gained solid matter, vacuum drying;
Step 4:Ammoniacal liquor is instilled into silver nitrate solution to solution clear, 20 are added in the silver nitrate solution by every liter of preparation The solid matter obtained in g steps 3, resulting solution is uniformly dispersed;
Step 5:Formaldehyde-alcohol-water mixed solution is prepared, the wherein volume ratio between formaldehyde, ethanol, water is 1:4:20;
Step 6:The solution that step 5 is prepared by volume 2:1 is added in step 4 resulting solution, lasting stirring, will react Solution is filtered afterwards, after deposit is cleaned through deionized water and ethanol, and vacuum drying obtains described covering material.
3. covering material as claimed in claim 2, it is characterised in that in step 1, the concentration of Tris aqueous slkalis is in 1-2 mg/ Between mL;The concentration of dispersion liquid is between 3-10 mg/mL.
4. covering material as claimed in claim 2, it is characterised in that in step 2, is at the uniform velocity stirred more than 24 hours.
5. covering material as claimed in claim 2, it is characterised in that in step 4, the concentration of silver nitrate solution is in 0.05-0.2 Between mol/L.
6. covering material as claimed in claim 2, it is characterised in that in step 6, is persistently stirred more than 2 hours.
7. the preparation method of the covering material as described in claim 1-6 is any.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108773842A (en) * 2018-09-07 2018-11-09 北京沃杰知识产权有限公司 A kind of preparation method and graphene of graphene
CN109631743A (en) * 2018-12-25 2019-04-16 东南大学 A kind of flexible strain transducer and preparation method thereof based on graphene nano silver

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Publication number Priority date Publication date Assignee Title
US6346136B1 (en) * 2000-03-31 2002-02-12 Ping Chen Process for forming metal nanoparticles and fibers
CN102614871A (en) * 2012-03-05 2012-08-01 天津大学 Method for preparing grapheme/silver nanoparticles composite material by using liquid phase method
CN103639421A (en) * 2013-12-04 2014-03-19 北京印刷学院 Preparation method for high-conductivity graphene and silver nanoparticle composite materials
CN104495811A (en) * 2014-12-12 2015-04-08 盐城市新能源化学储能与动力电源研究中心 Graphene composite material and preparation method thereof
CN105642135A (en) * 2016-03-23 2016-06-08 天津大学 Nano-silver particle functionalized graphene-based hybridized composite membrane, preparation and application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6346136B1 (en) * 2000-03-31 2002-02-12 Ping Chen Process for forming metal nanoparticles and fibers
CN102614871A (en) * 2012-03-05 2012-08-01 天津大学 Method for preparing grapheme/silver nanoparticles composite material by using liquid phase method
CN103639421A (en) * 2013-12-04 2014-03-19 北京印刷学院 Preparation method for high-conductivity graphene and silver nanoparticle composite materials
CN104495811A (en) * 2014-12-12 2015-04-08 盐城市新能源化学储能与动力电源研究中心 Graphene composite material and preparation method thereof
CN105642135A (en) * 2016-03-23 2016-06-08 天津大学 Nano-silver particle functionalized graphene-based hybridized composite membrane, preparation and application

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108773842A (en) * 2018-09-07 2018-11-09 北京沃杰知识产权有限公司 A kind of preparation method and graphene of graphene
CN108773842B (en) * 2018-09-07 2020-04-24 山东沃烯新材料科技有限公司 Preparation method of graphene and graphene
CN109631743A (en) * 2018-12-25 2019-04-16 东南大学 A kind of flexible strain transducer and preparation method thereof based on graphene nano silver

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