CN104174865B - Carbon parcel polyhedron Nano silver grain and the preparation method of controlled self assembly thereof - Google Patents
Carbon parcel polyhedron Nano silver grain and the preparation method of controlled self assembly thereof Download PDFInfo
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Abstract
The invention discloses carbon parcel polyhedron Nano silver grain and the preparation method of controlled self assembly thereof.Using a step hydrothermal technique, using glucose not only as reducing agent but also as carbon source, polyvinylpyrrolidone (PVP) is not only as the morphology control agent of argent growth but also cause compound particle self assembly.The step preparing carbon parcel polyhedron Nano silver grain is: 1.0 2.0g glucoses, 0.25 2.80gPVP and 0.02 0.04g silver nitrate is dissolved in 100mL deionized water successively, within ultrasonic 20 minutes, makes solid be completely dissolved.Taking 40mL mixed solution to be transferred in 50mL reactor, isothermal reaction 6 hours at a certain temperature in the range of 160 200 DEG C, product is cleaned, drying.The self assembly of nano-complex particle: other condition is constant, increases to certain value by PVP concentration, and the product suspension after cleaning is directly added drop-wise to carbon film, silicon chip or other carrier surface.The method process is simple, and low cost, it is easy to industrialization extends to other core-shell structure nanometer particle and the preparation of self-assembled structures and industrialized production.
Description
Technical field
The present invention relates to be applied to the noble metal nano particles pattern in the fields such as minitype optical device, waveguide and biological detection
Control and the preparation method of self assembly, especially the nuclear shell structure nano compound particle of one-step synthesis carbon parcel polyhedron Ag,
Or synchronize to realize this Ag/C compound particle self assembly；By regulation surfactant concentration, self assembly form is adjusted
Control.
Background technology
Noble metal nano particles is different from optical, electrical, the magnetic of bulk, is catalyzed and the character such as sensing, tool owing to showing many
There is boundless application prospect.These character are strongly depend on pattern and the size of particle, the therefore shape of metal nanoparticle
Looks control to have become one of current study hotspot.The preparation realizing specific morphology (such as polyhedron) noble metal nano particles is excellent
Change and the key of controlled material performance.But, due to small-size effect and high surface energy, exposed metal nanoparticle is in application
During oxidizable inefficacy.In order to solve this problem, particle surface cladding antioxidative material become effective way it
One.Owing to material with carbon element has chemical stability, biocompatibility and the electric conductivity etc. of excellence, carbon nano-encapsulated has incomparable
Advantage.The polyhedron metal nanoparticle that carbon to be obtained uniformly wraps up, the most all must be realized by multistep reaction, i.e. first
First prepare the single dispersing polyhedron metal nanoparticle with specific morphology, by solwution method, it is carried out surface carbon bag the most again
Wrap up in.Such process steps is loaded down with trivial details, and condition is harsh, relatively costly, and the product often heterogeneity (table of many metal nanoparticles
Face can not be wrapped, and the thickness of different particle clads also is difficult to uniformly), it is not readily converted into large-scale production.
The self assembly of metal nanoparticle is one of important channel realizing device.And, what particle assembling was constituted has
Sequence structure often shows many peculiar properties.Particularly, in ordered structure between particle, the interaction between particle and substrate
The light cooperative effect caused, the extreme enrichment optical property of metal nanoparticle so that it is at such as molecular recognition, molecule device
The aspect tools such as part, microsensor, thin-film optical filters, high sensitivity separation detection and surface is against corrosion, catalysis, electron transmission
There is broader practice prospect.But, due to the self assembly requirement to nanoparticle pattern, the most relevant metal nanoparticle is certainly
The report assembled is concentrated mainly on the particle with specific morphology (as bar-shaped and spherical etc.), the self assembly of polyhedron nanoparticle
Still rarely has report.Especially, a step realize the morphology control of metal nanoparticle, surface carbon nano-encapsulated and synchronize controlled from
Assemble and be still the difficult problem that material science workers face.
In recent years, hydro-thermal method has evolved into efficient, easy, the nano fabrication technique of low cost.Anti-by regulation hydro-thermal
The temperature answered, response time, solution ph etc., can be controlled the pattern of product, size and composition.So far,
Being related to one step hydro thermal method and prepare the report of organic polymer parcel nano silver wire, organic coating layer can protect silver nanoparticle well
Line kernel, prevents it from aoxidizing, but has no effect on electric conductivity.The present invention will develop a kind of new preparation method based on hydrothermal technique,
Realize the nano-complex particle of one-step synthesis carbon parcel polyhedron Ag, or one-step synthesis is by this Ag/C nuclear shell structure nano grain
The different dimensions self-assembled material that son builds.The method is to the development of nanotechnology, the device of metal nanoparticle and application
Industrialization has very important significance.
Summary of the invention
The purpose of the present invention: propose preparation method that is a kind of simple, quick, economic and that be suitable for, by regulation reaction solution
The parameters such as concentration, it is achieved one-step synthesis carbon wraps up the nuclear shell structure nano compound particle of polyhedron Ag, or synchronization realizes this
The controlled self assembly (self assembly of different dimensions) of Ag/C compound particle.The method overcome a step and realize the shape of Nano silver grain
Looks control, surface carbon is wrapped up and the technical barrier of controlled self assembly.
Technical scheme: carbon parcel polyhedron Nano silver grain and the preparation method of self-assembled structures thereof, it is special
Levying and be, using glucose not only as reducing agent but also as carbon source, polyvinylpyrrolidone (PVP) is both as the shape of argent growth
Looks controlling agent causes again compound particle self assembly.By change PVP concentration, can obtain carbon parcel single dispersing, have specific many
The Ag nanoparticle of face bodily form looks/carbon nucleocapsid structure composite nanoparticle, or synchronize realize this particle self assembly and
The control of assembling form.And, the thickness controllable of carbon nano-encapsulated layer.
The step preparing carbon parcel polyhedron Nano silver grain is: successively by 1.0-2.0g glucose, 0.25-0.75gPVP
It is dissolved in 100mL deionized water with 0.02-0.04g silver nitrate, within ultrasonic 20 minutes, makes solid and PVP be completely dissolved.Take 40mL to mix
Close solution to be transferred in 50mL reactor, isothermal reaction 6 hours at a certain temperature in the range of 160-200 DEG C.Reactor quilt
Naturally cooling to room temperature, product, through being centrifuged repeatedly, cleaning, finally dries in 50 ± 10 DEG C of baking ovens under vacuum or N2 protective atmosphere
Dry.Product is to be about polyhedron Ag nanoparticle (core) of 40-60nm by the length of side and carbon layer on surface (shell) is constituted.
The self assembly of Ag/C core-shell nano: other reaction condition is constant, increases to certain value by PVP concentration, cleans
After product suspension be directly added drop-wise to carbon film, silicon chip or other carrier surface.When PVP concentration reaches 0.07M, polyhedron
Ag/C self-assembly becomes 1-dimention nano chain structure；PVP concentration increases to 0.11M, Ag/C self-assembly and constitutes
Banded structure, its width about about 300nm；When PVP concentration is further up to 0.22M, Ag/C nanoparticle is assembled into arrangement
Orderly two-dimensional circle plate-like nanostructured.
Silver nitrate, glucose, PVP are dissolved in deionized water preparation reactant mixed solution.Room temperature or slightly above
Solution all can be prepared under room temperature condition.For making solid and PVP be completely dissolved, mixed solution needs ultrasonic 20 minutes.
Described hydro-thermal method, response time and reaction temperature all can be carried out in programme controlled isothermal reaction system.Hydro-thermal is anti-
Answering liquor capacity is 40mL, and filling rate is 80%, and optimal reaction temperature is 160-200 DEG C, and optimum reacting time is 6h.
The raw material that the preparation method of carbon parcel polyhedron Nano silver grain is used is cheap glucose and silver nitrate examination
Agent, the optimum condition of monodisperse particle to be obtained: concentration of glucose is 0.056-0.12M, silver nitrate concentration is 1.18-
2.35mM, PVP concentration 0.02-0.06M.Product is through being centrifuged repeatedly, cleaning, at vacuum or N250 ± 10 DEG C of drying under atmosphere,
Drying time is more than 6 hours.
Other reaction condition is constant, when PVP concentration meets and exceeds 0.07M, can realize Ag/C nanoparticle from group
Dress.All can obtain at carbon film, silicon chip or other carrier surface.
The hydro-thermal method of the present invention need not any template, and step is simple, a step realize Ag/C core-shell structure nanometer particle and
The preparation of self-assembled structures, overcomes template (such as electrochemical deposition, chemical gaseous phase deposition) and multistep processes is complicated, cost is high
Shortcoming.Product is to be made up of the length of side about 40-60nm polyhedron Ag particle (core) and carbon layer on surface (shell).Being coated with beneficially of carbon
Prevent the oxidation of nanometer galactic nucleus, corrosion, thus improve its chemical reactivity and heat stability.Additionally, self-assembled structures performance
Go out excellence optical property, such as molecular device, microsensor, thin-film optical filters, high sensitivity separation detection and
The aspects such as surface is against corrosion, catalysis, electron transmission have broad prospect of application.The method experimental provision is simple, easy and simple to handle, controlled
Property is good, easily accomplish scale production, and especially has the strongest suitability, extends to other metal system.
Beneficial effects of the present invention:
(1) method disclosed by the invention can be used to prepare crystallite dimension is nano level Ag/C nucleocapsid structure compound particle,
Galactic nucleus is polyhedron, and the length of side is about 40-60nm, even size distribution；And synchronize to realize the self assembly of different dimensions；
(2) using cheap glucose, silver nitrate and PVP is raw material, and step is simple, and cost is relatively low；
(3) the invention discloses a kind of simple, quick, economic and that different dimensions can be applicable to nucleocapsid structure and be combined grain
The syntheti c route of sub-self-assembled material；Overcome the shortcoming that traditional preparation methods operation complexity, complex steps and cost are high.
(4) other preparation method (such as sol-gal process) compares, the feature of hydro-thermal method:
1. experimental provision, experiment condition and preparation process are simple, easily operate, and the productivity of material is high；
2. controllability is good, can be controlled the feature of product by regulation solution concentration, heat treatment temperature and time；
The most with low cost, easily realize, there is good industrial applications prospect；
4. the suitability is strong, extends to other metal.
(5) compared with pure silver nanoparticles, the particular advantages that the product of this patent of invention has:
1. carbon cladding can prevent the reunion of nano metal, aoxidizes and corrode, thus improves its chemical reactivity and heat is steady
Qualitative；
2. the ordered structure of self assembly shows the optical property of excellence, can operate with microdevice and novel light absorbs material
Material etc..
Accompanying drawing illustrates:
Fig. 1 is representative experiment (glucose 0.07M, PVP concentration 0.04M, silver nitrate 0.25mM, react 6h by 180 DEG C) institute
Prepare SEM figure (A) and XRD figure spectrum (B) of product.
Fig. 2 is TEM figure (A) of product shown in Fig. 1, and TEM (B) and the HRTEM figure of single representative Ag/C core-shell particles (is inserted
Figure).
Fig. 3 is that other condition is constant, and the response time is respectively the digital photograph of the obtained product of 1h, 2h, 3h, 4h and 5h
And corresponding uv-visible absorption spectra figure (B) (A).
Fig. 4 is that reaction condition is identical with representative experiment, and PVP concentration is respectively 0.07M (A), 0.11M (B) and 0.22M
(C) the TEM figure of prepared product under the conditions of；D is the further amplification of C figure.
Fig. 5 is digital photograph (A) and corresponding uv-visible absorption spectrum figure (B), wherein a, b, c of product shown in Fig. 4
PVP concentration be 0.07M, 0.11M and 0.22M.
Detailed description of the invention
In the present invention, hydro-thermal method prepares carbon parcel polyhedron Nano silver grain and the detailed description of the invention of self-assembled structures thereof
As follows:
Embodiment 1
The preparation of Ag/C nucleocapsid structure compound particle: successively 1.25g glucose, 0.50gPVP and 0.028g silver nitrate are depended on
The secondary 100ml of being dissolved in deionized water obtains reaction mixture, within ultrasonic 20 minutes, makes solid and PVP be completely dissolved.Solutions Solution
The concentration of middle glucose, PVP and silver nitrate is respectively 0.07M, 0.04M and 0.25mM.Take 40ml mixed solution and be transferred to 50ml
In reactor, react 6 hours under 180 DEG C of constant temperatures.Reactor is naturally cooled to room temperature, product through being centrifuged repeatedly, clearly
Wash, finally at vacuum or N2Under protective atmosphere, 50 ± 10 DEG C of baking ovens are dried.
Fig. 1 (A) is the SEM figure of product prepared by embodiment 1, it can be seen that a large amount of mono-dispersed nano particles are formed.By
The SEM illustration of high-amplification-factor is it can be seen that nanoparticle presents uniform polyhedron pattern, and the length of side is about 40-60nm.Fig. 1
(B) be this product XRD figure spectrum, stronger diffraction maximum shows that product has good crystallinity, the position of diffraction maximum and the center of area
The diffraction maximum of cubic structure silver is completely the same.The wider faint diffraction maximum in 22 ° of (2 θ) places belongs to the amorphous characteristic of carbon encapsulating layer
Peak.XRD result shows that product is the polyhedron Nano silver grain that carbon parcel has high crystalline.
Fig. 2 (A) is the TEM picture of product shown in Fig. 1, it can be seen that nanoparticle is polyhedron pattern, has well
Homogeneity and monodispersity, this is consistent with the SEM result of Fig. 1.Fig. 2 (B) is the TEM figure of single representative composite particle, bright
Aobvious contrast shows that kernel is metal Ag, and top layer is carbon.The polygonal length of side is averagely about 45nm, carbon integument thickness about 5-
10nm, further demonstrate that the nucleocapsid structure of Ag/C compound particle.The nano-particles size numerical value measured by TEM characterizes with SEM
Result consistent.Meanwhile, in illustration HRTEM, the multiple twin structure of display also show the polyhedron knot of silver kernel nanoparticle
Structure feature.
Embodiment 2
Response time changes 1 hour into.Other conditions are with embodiment 1.
Embodiment 3
Response time changes 2 hours into.Other conditions are with embodiment 1.
Embodiment 4
Response time changes 4 hours into.Other conditions are with embodiment 1.
Embodiment 5
Response time changes 5 hours into.Other conditions are with embodiment 1.
Fig. 3 (A) is that reaction mixture concentration is constant, and reaction is 180.Hydro-thermal reaction 1h at DEG C, 2h, 4h, 5h are obtained
The photo of product aqueous suspension.It is found that the color of product aqueous solution with the response time increase and by milky to deeply
Brown gradually alternation.Fig. 3 (B) is corresponding uv-visible absorption spectrum figure, and the absworption peak position of response time 1-4h is about
284nm, absworption peak position does not occur substantially to offset；Response time be the absworption peak position of 5h be 279nm, to shortwave skew be
5nm.Time thus it could be speculated that reaction proceeds to 5h, the corner angle of particle surface are the most prominent, result in the change of characteristic absorption peak position
Change.
Embodiment 6
In reaction mixture, PVP content is 0.02M, and other conditions are with embodiment 1.
Embodiment 7
In reaction mixture, PVP content is 0.06M, and other conditions are with embodiment 1.
Embodiment 8
In reaction mixture, PVP content is 0.07M, and other conditions are with embodiment 1.
Embodiment 9
In reaction mixture, PVP content is 0.11M, and other conditions are with embodiment 1.
Embodiment 10
In reaction mixture, PVP content is 0.18M, and other conditions are with embodiment 1.
Embodiment 11
In reaction mixture, PVP content is 0.22M, and other conditions are with embodiment 1.
When Fig. 4 is that in reaction mixture, Ag and concentration of glucose are constant, PVP concentration be respectively 0.07M (embodiment 8),
The TEM figure of product prepared by 0.11M (embodiment 9), 0.22M (embodiment 11) next step hydro-thermal method.It will be seen that when PVP is dense
When degree and 0.04M increase to 0.07M, product is become 1-dimention nano by monodispersed polyhedron Ag/C nanoparticle (Fig. 1 and Fig. 2)
The package assembly (Fig. 4 A) of chain.Increase PVP concentration is to 0.11M (embodiment 9) further, is made up of Ag/C self-assembly
One-dimensional banded structure generate, the width of nano belt reaches about 300nm, as shown in Fig. 4 (B).When PVP concentration reaches 0.22M
Time (embodiment 11), Ag/C nanoparticle is assembled into the orderly two-dimensional nano disc structure (Fig. 4 C) of arrangement.Along with PVP content
Increasing, the ordering degree of nano belt can improve further.Therefore, PVP is to Ag/C core-shell nano to varying degrees
Assembling serves key effect.
Fig. 5 (A) is the digital photograph obtaining product aqueous suspension under the different PVP concentration shown in Fig. 4.It will be seen that
Solution colour with the increase of PVP concentration by yellow to bottle green alternation, this be the Ag/C nanoparticle that causes due to PVP from group
The form of dress is different (see Fig. 4), and the close nano-sized silver particle surface phasmon leaned on each other interacts, and this makes not
Different collective effects is produced with the form of assembling.Fig. 5 (B) is corresponding uv-visible absorption spectrum figure, and absworption peak is mainly concentrated
In visible region.Along with being gradually increased of PVP concentration, maximum absorption band occurs respectively at 548nm, 511nm and 452nm, i.e.
Peak position is to short-wave band generation apparent motion.
Claims (9)
1. the preparation method of carbon parcel polyhedron Nano silver grain, it is characterised in that: glucose is not only as reducing agent but also make
For carbon source, polyvinylpyrrolidone is not only as the morphology control agent of argent growth but also cause compound particle self assembly；Concrete step
Suddenly it is: successively 1.0-2.0g glucose, 0.25-0.75g polyvinylpyrrolidone and 0.02-0.04g silver nitrate are dissolved in 100mL
In deionized water, within ultrasonic 20 minutes, make solid and polyvinylpyrrolidone be completely dissolved, obtain mixed solution；Take 40mL mixing molten
Liquid is transferred in 50mL reactor, isothermal reaction 6 hours in the range of 160-200 DEG C；Reactor is naturally cooled to room temperature, produces
Thing is through being centrifuged repeatedly, cleaning, finally at vacuum or N2Under protective atmosphere, 50 ± 10 DEG C of baking ovens are dried.
The preparation method of carbon the most according to claim 1 parcel polyhedron Nano silver grain, it is characterised in that: described reaction
The filling rate of still is 80%.
The preparation method of carbon the most according to claim 1 parcel polyhedron Nano silver grain, it is characterised in that: described drying
Time be more than 6 hours.
The preparation method of carbon the most according to claim 1 parcel polyhedron Nano silver grain, the Portugal in described mixed solution
Grape sugar concentration is 0.056-0.12M, and the silver nitrate concentration in described mixed solution is 1.18-2.35mM, in described mixed solution
Polyvinylpyrrolidoneconcentration concentration 0.02-0.06M.
The preparation method of carbon the most according to claim 1 parcel polyhedron Nano silver grain, it is characterised in that: obtained
Carbon parcel polyhedron Nano silver grain is 40-60nm polyhedron Ag nanoparticle by the length of side and carbon layer on surface is constituted；Described multiaspect
Body Ag nanoparticle has specific polyhedron pattern, and described carbon layer on surface is as shell, the thickness controllable of described carbon layer on surface.
6. the preparation method of an Ag/C core-shell nano self-assembled structures, it is characterised in that: glucose is both as reducing agent
Again as carbon source, polyvinylpyrrolidone is not only as the morphology control agent of argent growth but also cause compound particle self assembly；Tool
Body step is: successively by 1.0-2.0g glucose, pyrrolidone given a tongue-lashing by 0.25-0.75g polyethylene and 0.02-0.04g silver nitrate is dissolved in
In 100mL deionized water, within ultrasonic 20 minutes, make solid and polyvinylpyrrolidone be completely dissolved, obtain mixed solution；Take 40mL
Mixed solution is transferred in 50mL reactor, isothermal reaction 6 hours in the range of 160-200 DEG C；Reactor be naturally cooled to
Room temperature, product, through being centrifuged repeatedly, cleaning, obtains product suspension；When polyvinylpyrrolidoneconcentration concentration is more than 0.07M, will be clear
Product suspension after washing directly is added drop-wise to carbon film or silicon chip surface, obtains Ag/C core-shell nano self-assembled structures.
The preparation method of Ag/C core-shell nano self-assembled structures the most according to claim 6, it is characterised in that: work as institute
Stating the polyvinylpyrrolidoneconcentration concentration in mixed solution when reaching 0.07M, Ag/C core-shell nano self-assembled structures is one-dimensional
Nano chain structure；When the polyvinylpyrrolidoneconcentration concentration in described mixed solution reaches 0.11M, Ag/C core-shell nano is certainly
Package assembly is banded structure, and the width of described banded structure is 300nm；Polyvinylpyrrolidone in described mixed solution
When concentration reaches 0.22M, Ag/C core-shell nano self-assembled structures is the two-dimensional circle plate-like nanostructured that arrangement is orderly.
The preparation method of Ag/C core-shell nano self-assembled structures the most according to claim 6, it is characterised in that: described
The filling rate of reactor is 80%.
The preparation method of Ag/C core-shell nano self-assembled structures the most according to claim 6, it is characterised in that: described
Concentration of glucose in mixed solution is 0.056-0.12M, and the silver nitrate concentration in described mixed solution is 1.18-2.35mM.
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| CN105798289B (en) * | 2014-12-31 | 2019-02-19 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method and applications for the noble metal nano particles that carbon is shell isolated |
| CN106475022B (en) * | 2015-09-02 | 2019-09-27 | 南京理工大学 | A kind of active antibacterial microballoon and preparation method thereof |
| CN105717091B (en) * | 2016-01-29 | 2019-01-18 | 南京理工大学 | A kind of SERS substrate of persistent high efficiency and preparation method thereof |
| CN108264016A (en) * | 2017-12-26 | 2018-07-10 | 中国科学院合肥物质科学研究院 | A kind of diverse nano structure composite array and preparation method thereof |
| CN108568519B (en) * | 2018-05-21 | 2020-01-17 | 江汉大学 | Preparation method and application of silver nano composite material |
| CN109909493A (en) * | 2019-02-25 | 2019-06-21 | 华中科技大学 | A kind of method that electron beam irradiation improves metal material stability |
| CN113909486B (en) * | 2021-07-23 | 2024-02-23 | 徐州工程学院 | Preparation method of ferroferric oxide loaded carbon-based thin film gold nanocomposite particles |
| CN113698828B (en) * | 2021-08-24 | 2022-12-30 | 南京大学 | Preparation method of anti-corrosion coating material based on carbon-coated silver nanospheres |
| CN114160806A (en) * | 2021-12-02 | 2022-03-11 | 深圳市华科创智技术有限公司 | Core-shell structure silver nanoparticles prepared by biomass reduction and preparation method thereof |
| CN114713813B (en) * | 2022-03-24 | 2023-03-10 | 厦门大学 | Carbon-coated gold/silver nano particle for photovoltaic power generation and synthesis method thereof |
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