CN107999782A - A kind of preparation method of electrum hollow polyhedral - Google Patents
A kind of preparation method of electrum hollow polyhedral Download PDFInfo
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- CN107999782A CN107999782A CN201711098009.0A CN201711098009A CN107999782A CN 107999782 A CN107999782 A CN 107999782A CN 201711098009 A CN201711098009 A CN 201711098009A CN 107999782 A CN107999782 A CN 107999782A
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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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0549—Hollow particles, including tubes and shells
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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 discloses a kind of preparation method of electrum hollow polyhedral, including：Silver nanocubes are prepared in 150~195 DEG C of oil baths using polyol reduction method；The silver nanocubes are distributed in surfactant solution, so as to obtain the silver nanocubes of surfactant-dispersed；Reducing agent and the gold chloride of surfactant-dispersed are sequentially added into the silver nanocubes of the surfactant-dispersed, it is centrifuged after reaction 10min~2h, the particle obtained after centrifugation is washed again, so that electrum hollow polyhedral be made.The present invention can be made gold and silver Elemental redistribution uniformly as template using silver nanocubes and not replicate the hollow polyhedral of template pattern, and the wall of the hollow polyhedral is thicker, solid non-breakable.
Description
Technical field
The present invention relates to electrum technical field of nanometer material preparation, more particularly to a kind of electrum hollow polyhedral
Preparation method.
Background technology
Optical property-local surface plasma resonance of noble metal nano particles is obviously dependent on the size of particle, group
Into the environment of, shape and surrounding, have in photoelectric device, Surface-enhanced spectroscopic and biological medicine etc. and potentially should
With value.Compared to the nano material of single metal, binary metal nano-particle has only in optics, catalysis, electronics etc.
Special advantage, therefore binary metal nano-particle increasingly causes the concern of researcher.
At present, people can prepare the binary metal nanometer of core shell structure or alloy structure by a variety of distinct methods
Particle.Due to gold and silver, both noble metals have substantial amounts of free electron, gold and silver when being subject to light to excite, can produce compared with
Strong plasma resonance, and cause Surface enhanced Raman scattering, this causes the nanometer that people form gold and silver both metals
Particle is interested.Core shell structure gold silver nanometer particle largely still has obvious golden or silver-colored spy
Property, and utilize alloy structure gold silver nanometer particle (i.e. gold-silver alloy nano particle) made from displacement reaction can be in atomic level
Realize the dispersed of gold and silver element, and this gold-silver alloy nano particle is usually hollow-core construction, and this has than solid construction
There is the specific surface area of bigger.In addition, in the prior art, utilize gold-silver alloy nano particle, its pattern made from displacement reaction
Usually limited be subject to the pattern of original silver-colored template, such as：Obtained as template using nano silver wire is electrum nanotube, with
Silver nanoparticle ball for template it is obtained be electrum hollow ball, obtained as template using silver nanocubes is electrum
Hollow cube.But obtained gold-silver alloy nano particle is reacted using displacement in the prior art, its pattern replicates mostly
The pattern of template is sacrificed, and the wall of its hollow-core construction is extremely easily broken than relatively thin.
The content of the invention
In order to solve the wall of gold-silver alloy nano particle its hollow-core construction obtained by existing preparation method than relatively thin, very
The technical problem being easily broken, can be with silver nanoparticle the present invention provides a kind of preparation method of electrum hollow polyhedral
The uniform electrum hollow polyhedral of gold and silver Elemental redistribution is made for template in cube, is specially hollow truncated cube, and
It is solid non-breakable and the wall of the hollow polyhedral is thicker.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of preparation method of electrum hollow polyhedral, comprises the following steps：
Step A, silver nanocubes are prepared in 150~195 DEG C of oil baths using polyol reduction method；
Step B, the silver nanocubes are distributed in surfactant solution, so as to obtain surfactant-dispersed
Silver nanocubes；
Step C, reducing agent and surfactant are sequentially added into the silver nanocubes of the surfactant-dispersed
Scattered gold chloride, is centrifuged after reacting 10min~2h, then the solid to being obtained after centrifugation washs, from
And electrum hollow polyhedral is made.
Preferably, every 20~200uL silver nanocubes use the reducing agent that 0.1~5mL concentration is 0.01~1mol/L
With the gold chloride of 0.1~5mL surfactant-disperseds；Wherein, in the gold chloride of the surfactant-dispersed gold chloride it is dense
Spend for 0.1~0.5mmol/L.
Preferably, the reducing agent is using in citric acid, sodium citrate, potassium citrate, ascorbic acid, sodium ascorbate
At least one.
Preferably, it is described to sequentially add reducing agent and surface into the silver nanocubes of the surfactant-dispersed
The gold chloride that activating agent disperses includes：Reduction is added into the silver nanocubes of the surfactant-dispersed while stirring
Agent, then stirs 2~10min, adds the gold chloride of surfactant-dispersed.
Preferably, in the silver nanocubes of the surfactant-dispersed concentration of surfactant for 0.02~
0.2mol/L；The concentration of surfactant is 0.02~0.2mol/L in the gold chloride of the surfactant-dispersed.
Preferably, the surfactant is using polyvinylpyrrolidone, cetyl trimethylammonium bromide, hexadecane
At least one of base trimethyl ammonium chloride, lauryl sodium sulfate, halogenated phosphates.
Preferably, it is described washing is carried out to the solid that is obtained after centrifugation to include：Using distilled water and absolute ethyl alcohol
The solid obtained after centrifugation is washed multiple.
Preferably, the use polyol reduction method prepares silver nanocubes in 150~195 DEG C of oil baths includes
Following steps：
Step A1, silver nitrate solution, concentration that concentration is 10~50mg/mL are respectively configured by solvent of 1,5- pentanediols is
The polyvinylpyrrolidonesolution solution and concentration of 10~50mg/mL is the anhydrous cupric chloride solution of 10~50mg/mL, and by the nothing
Water copper chloride solution is distributed in the silver nitrate solution, so as to obtain the silver nitrate solution containing anhydrous cupric chloride；
Step A2,1,5-PD is taken in reaction vessel, and is placed in 150~195 DEG C of oil baths, with 200~
The speed stirring of 300r/min, is allowed to thermally equivalent, keeps the temperature 10~30min, step is then alternately added into the reaction vessel
Silver nitrate solution and polyvinylpyrrolidonesolution solution containing anhydrous cupric chloride in rapid A1, the speed of addition is 50~200uL/
Min, the number of addition is 16~22 times；
Step A3, after adding completely, the reaction vessel is taken out, is cooled to room temperature while stirring, then to described anti-
The solution in container is answered to be washed, so as to prepare silver nanocubes.
As seen from the above technical solution provided by the invention, the system of electrum hollow polyhedral provided by the invention
Preparation Method is using silver nanocubes made from polyol reduction method as raw material, and by being stood to the silver nanoparticle of surfactant-dispersed
The weaker reducing agent of reproducibility and the gold chloride of surfactant-dispersed are sequentially added in cube, and to each material concentration, use
Amount and the control in reaction time, so that the finally equally distributed electrum hollow polyhedral of obtained gold and silver element, and should
The wall of hollow-core construction is thicker, solid non-breakable.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, without creative efforts, other can also be obtained according to these attached drawings
Attached drawing.
Fig. 1 is the stereoscan photograph and absorption curves schematic diagram of the silver nanocubes in the embodiment of the present invention 3.
Fig. 2 is the stereoscan photograph and difference of final obtained electrum hollow polyhedral in the embodiment of the present invention 3
Angular transmission electromicroscopic photograph.
Embodiment
With reference to the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Ground describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained without making creative work
Example, belongs to protection scope of the present invention.
The preparation method of electrum hollow polyhedral provided by the present invention is described in detail below.It is of the invention real
Apply the content not being described in detail in example and belong to the prior art known to professional and technical personnel in the field.
A kind of preparation method of electrum hollow polyhedral, includes the following steps：
Step A, silver nanocubes are prepared in 150~195 DEG C of oil baths using polyol reduction method.
Step B, the silver nanocubes are distributed in surfactant solution, so as to obtain surfactant-dispersed
Silver nanocubes.
Step C, reducing agent and surfactant are sequentially added into the silver nanocubes of the surfactant-dispersed
Scattered gold chloride, is centrifuged after reacting 10min~2h, then the solid to being obtained after centrifugation washs, from
And electrum hollow polyhedral is made.
Specifically, each step of the preparation method of the electrum hollow polyhedral can include embodiments below：
(1) in step, the use polyol reduction method prepares silver nanoparticle cube in 150~195 DEG C of oil baths
Body may comprise steps of：
It is 10~50mg/mL (preferably 20mg/mL) that 1. concentration step A1, is respectively configured by solvent of 1,5- pentanediols
Silver nitrate solution, concentration be the polyvinylpyrrolidonesolution solution of 10~50mg/mL (preferably 20mg/mL) and concentration be 10~
The anhydrous cupric chloride solution of 50mg/mL (preferably 10mg/mL), and the anhydrous cupric chloride solution is distributed to the silver nitrate
In solution, so as to obtain the anhydrous cupric chloride solution that silver nitrate disperses.
2. step A2, taking the 1,5-PD of 2.5~10mL (preferably 5mL) in reaction vessel, and it is placed on 150
In~195 DEG C of (preferably 175 DEG C) oil baths, stirred with the speed of 200~300r/min (preferably 280r/min), be allowed to uniform
Heated, 10~30min of insulation (preferably 20min), is then alternately added silver nitrate point in step A1 into the reaction vessel
Scattered anhydrous cupric chloride solution and polyvinylpyrrolidonesolution solution, the speed of addition is 50~200uL/min (preferably 125uL/
Min), the number of addition is 16~22 times (preferably 18 times).
3. after step A3, adding completely, the reaction vessel is taken out, is cooled to room temperature while stirring, then by described in
Solution in reaction vessel is washed for several times, so as to prepare silver nanocubes using distilled water and absolute ethyl alcohol.
(2) in stepb, the concentration of surfactant is 0.02 in the silver nanocubes of the surfactant-dispersed
~0.2mol/L (preferably 0.05mol/L)；And the surfactant can use polyvinylpyrrolidone (PVP), 16
Alkyl trimethyl ammonium bromide (CTAB), hexadecyltrimethylammonium chloride (CTAC), lauryl sodium sulfate (SDS), chloro ten
At least one of six alkyl pyridines (CPC).
(3) in step C, reduction is preferably added into the silver nanocubes of the surfactant-dispersed while stirring
Agent, then stirs 2~10min (preferably 5min), adds the gold chloride of surfactant-dispersed, question response 10min~2h
It is centrifuged after (preferably 30min), then the solid obtained after centrifugation is washed using distilled water and absolute ethyl alcohol
Repeatedly, so that electrum hollow polyhedral be made.Wherein, every 20~200uL silver nanocubes use 0.1~5mL concentration
For the reducing agent of 0.01~1mol/L and the gold chloride of 0.1~5mL surfactant-disperseds, preferably every 50uL silver nanoparticles cube
Body uses the reducing agent and the gold chloride of 1mL surfactant-disperseds that 1mL concentration is 0.1mol/L；The surfactant-dispersed
Gold chloride in the concentration of gold chloride be for 0.1~0.5mmol/L (preferably 0.1mmol/L), the concentration of surfactant
0.02~0.2mol/L (preferably 0.05mol/L).In practical applications, the reducing agent can use and citric acid, lemon
At least one of close reducing agent of sour sodium, potassium citrate, the reproducibility of ascorbic acid or sodium ascorbate；The surface
Activating agent can use polyvinylpyrrolidone (PVP), cetyl trimethylammonium bromide (CTAB), cetyl trimethyl chlorination
At least one of ammonium (CTAC), lauryl sodium sulfate (SDS), halogenated phosphates (CPC).
Compared with prior art, the preparation method of the electrum hollow polyhedral in the present invention at least has following excellent
Point：
(1) shape of template is replicated mostly using its pattern of gold-silver alloy nano particle made from displacement reaction in the prior art
Looks；And although the preparation method of electrum hollow polyhedral provided by the invention is using silver nanocubes as template and utilizes
Prepared by displacement reaction, but obtained gold-silver alloy nano particle, its pattern are hollow truncated cube (i.e. not backed stampers
The hollow polyhedral of plate pattern) structure, and contain two kinds of metals of gold and silver at the same time, gold and silver Elemental redistribution is uniform.
(2) in the prior art the wall of obtained its hollow-core construction of gold-silver alloy nano particle than it is relatively thin (typically smaller than
10nm), and its wall surface is usually discontinuous, and according to the difference of extent of corrosion, its wall surface usually has various sizes of hole,
And the electrum hollow polyhedral obtained by the preparation method of electrum hollow polyhedral provided by the invention its hollow knot
The wall of structure is thicker (being at least 15nm, sometimes even over 100nm), and its wall surface is continuous, therefore solid is not easy
It is broken.
(3) compared with silver nano-grain simple in the prior art, electrum hollow polyhedral provided by the invention
Electrum hollow polyhedral stability increase obtained by preparation method, and the specific surface area with bigger.With existing skill
Simple gold nano grain is compared in art, the gold and silver obtained by the preparation method of electrum hollow polyhedral provided by the invention
Alloy hollow polyhedron cost reduction.Therefore the gold obtained by the preparation method of electrum hollow polyhedral provided by the invention
Silver alloy hollow polyhedral make use of the cooperative effect between two kinds of metals, can obtain more excellent performance.
To sum up, using silver nanocubes as template gold and silver Elemental redistribution can be made uniformly and not in the embodiment of the present invention
The hollow polyhedral for sacrificing template pattern is replicated, and the wall of the hollow polyhedral is thicker, it is solid non-breakable.
In order to more clearly from show technical solution provided by the present invention and caused technique effect, below with tool
The preparation method for the electrum hollow polyhedral that body embodiment provides the embodiment of the present invention is described in detail.
Embodiment 1
A kind of preparation method of electrum hollow polyhedral, includes the following steps：
Step a1, it is that solvent is respectively configured concentration and is as the silver nitrate solution of 20mg/mL, concentration using 1,5- pentanediols
The polyvinylpyrrolidonesolution solution and concentration of 20mg/mL is the anhydrous cupric chloride solution of 20mg/mL, and by the anhydrous cupric chloride
Solution is distributed in the silver nitrate solution, so as to obtain the anhydrous cupric chloride solution that silver nitrate disperses.
Step b1, the 1,5-PD of 5mL is taken in single port vial, and is placed in 175 DEG C of oil baths, with 280r/
The speed stirring of min, is allowed to thermally equivalent, keeps the temperature 20min, be then alternately added nitre in step a1 into the single port vial
The scattered anhydrous cupric chloride solution of sour silver and polyvinylpyrrolidonesolution solution, the speed of addition are 125uL/min, the number of addition
For 18 times.
Step c1, after adding completely, the single port vial is taken out, is cooled to room temperature while stirring, then by described in
Solution in single port vial is washed for several times, so as to prepare silver nanocubes using distilled water and absolute ethyl alcohol.
Step d1, silver nanocubes described in 50uL are distributed to the cetyl trimethyl chlorine that concentration is 0.05mol/L
Change in ammonium salt solution, so as to obtain the silver nanocubes that 1mL hexadecyltrimethylammonium chlorides disperse.
Step e1,1mL is added in the silver nanocubes disperseed while stirring to the hexadecyltrimethylammonium chloride
Concentration is the ascorbic acid of 0.1mol/L, then stirs 5min, adds the hexadecane that 1mL gold chlorides concentration is 0.01mmol/L
The gold chloride that base trimethyl ammonium chloride disperses, is centrifuged after question response 30min, then using distilled water and absolute ethyl alcohol pair
The solid washing obtained after centrifugation is multiple, so that electrum hollow polyhedral be made.
Embodiment 2
A kind of preparation method of electrum hollow polyhedral, includes the following steps：
Step a2, it is that solvent is respectively configured concentration and is as the silver nitrate solution of 20mg/mL, concentration using 1,5- pentanediols
The polyvinylpyrrolidonesolution solution and concentration of 20mg/mL is the anhydrous cupric chloride solution of 20mg/mL, and by the anhydrous cupric chloride
Solution is distributed in the silver nitrate solution, so as to obtain the anhydrous cupric chloride solution that silver nitrate disperses.
Step b2, the 1,5-PD of 5mL is taken in single port vial, and is placed in 175 DEG C of oil baths, with 280r/
The speed stirring of min, is allowed to thermally equivalent, keeps the temperature 20min, be then alternately added nitre in step a2 into the single port vial
The scattered anhydrous cupric chloride solution of sour silver and polyvinylpyrrolidonesolution solution, the speed of addition are 125uL/min, the number of addition
For 18 times.
Step c2, after adding completely, the single port vial is taken out, is cooled to room temperature while stirring, then by described in
Solution in single port vial is washed for several times, so as to prepare silver nanocubes using distilled water and absolute ethyl alcohol.
Step d2, silver nanocubes described in 50uL are distributed to the cetyl trimethyl bromine that concentration is 0.05mol/L
Change in ammonium salt solution, so as to obtain the silver nanocubes that 1mL cetyl trimethylammonium bromides disperse.
Step e2,1mL is added in the silver nanocubes disperseed while stirring to the cetyl trimethylammonium bromide
Concentration is the ascorbic acid of 0.1mol/L, then stirs 5min, adds the hexadecane that 1mL gold chlorides concentration is 0.01mmol/L
The gold chloride that base trimethylammonium bromide disperses, is centrifuged after question response 30min, then using distilled water and absolute ethyl alcohol pair
The solid washing obtained after centrifugation is multiple, so that electrum hollow polyhedral be made.
Embodiment 3
A kind of preparation method of electrum hollow polyhedral, includes the following steps：
Step a3, it is that solvent is respectively configured concentration and is as the silver nitrate solution of 20mg/mL, concentration using 1,5- pentanediols
The polyvinylpyrrolidonesolution solution and concentration of 20mg/mL is the anhydrous cupric chloride solution of 20mg/mL, and by the anhydrous cupric chloride
Solution is distributed in the silver nitrate solution, so as to obtain the anhydrous cupric chloride solution that silver nitrate disperses.
Step b3, the 1,5-PD of 5mL is taken in single port vial, and is placed in 175 DEG C of oil baths, with 280r/
The speed stirring of min, is allowed to thermally equivalent, keeps the temperature 20min, be then alternately added nitre in step a3 into the single port vial
The scattered anhydrous cupric chloride solution of sour silver and polyvinylpyrrolidonesolution solution, the speed of addition are 125uL/min, the number of addition
For 18 times.
Step c3, after adding completely, the single port vial is taken out, is cooled to room temperature while stirring, then by described in
Solution in single port vial is washed for several times, so as to prepare silver nanocubes using distilled water and absolute ethyl alcohol.
Step d3, silver nanocubes described in 50uL are distributed to the halogenated phosphates that concentration is 0.05mol/L
In solution, so as to obtain the silver nanocubes that 1mL halogenated phosphates disperse.
Step e3,1mL concentration is added in the silver nanocubes disperseed while stirring to the halogenated phosphates
For the ascorbic acid of 0.1mol/L, 5min is then stirred, adds the chloro-hexadecane that 1mL gold chlorides concentration is 0.01mmol/L
The gold chloride that yl pyridines disperse, is centrifuged after question response 30min, then using distilled water and absolute ethyl alcohol to centrifuging
The solid washing obtained afterwards is multiple, so that electrum hollow polyhedral be made.
Specifically, following pattern and performance detection are carried out in 3 implementation process of the embodiment of the present invention：
(1) morphology observation is carried out to silver nanocubes made from step c3 in the embodiment of the present invention 3 and photo absorption performance is examined
Survey, so as to obtain the stereoscan photograph and absorption curves schematic diagram of silver nanocubes as shown in Figure 1；Wherein, Fig. 1 a
For the stereoscan photograph of silver nanocubes made from step c3 in the embodiment of the present invention 3, Fig. 1 b are in the embodiment of the present invention 3
The absorption curves schematic diagram of silver nanocubes made from step c3.As seen from Figure 1：The size of silver-colored cubic granules is about
For 125 ± 5nm, the absworption peak of light absorbs is located at 482nm and has several corresponding acromions, is the suction of typical cubic granules
Receive peak.
(2) morphology observation is carried out to electrum hollow polyhedral made from step e3 in the embodiment of the present invention 3, so that
To the stereoscan photograph and different angle transmission electron microscope photo of electrum hollow polyhedral as shown in Figure 2；Wherein, Fig. 2 a
For the stereoscan photograph of electrum hollow polyhedral made from step e3 in the embodiment of the present invention 3, Fig. 2 b, Fig. 2 c, Fig. 2 d
For the different angle transmission electron microscope photo of electrum hollow polyhedral made from step e3 in the embodiment of the present invention 3.Can by Fig. 2
To find out：Cube structure compared to Fig. 1, the structure in Fig. 2 are changed into hollow truncated cube (i.e. hollow polyhedral) knot
Structure, and the wall thickness of the structure is about 40nm.
To sum up, using silver nanocubes as template gold and silver Elemental redistribution can be made uniformly and not in the embodiment of the present invention
The hollow polyhedral of template pattern is replicated, and the wall of the hollow polyhedral is thicker, it is solid non-breakable.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can readily occur in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (8)
1. a kind of preparation method of electrum hollow polyhedral, it is characterised in that comprise the following steps：
Step A, silver nanocubes are prepared in 150~195 DEG C of oil baths using polyol reduction method；
Step B, the silver nanocubes are distributed in surfactant solution, so as to obtain the silver of surfactant-dispersed
Nanocube；
Step C, reducing agent and surfactant-dispersed are sequentially added into the silver nanocubes of the surfactant-dispersed
Gold chloride, be centrifuged after reacting 10min~2h, then the solid to being obtained after centrifugation washs, so as to make
Obtain electrum hollow polyhedral.
2. the preparation method of electrum hollow polyhedral according to claim 1, it is characterised in that every 20~200uL
Silver nanocubes use the reducing agent and 0.1~5mL surfactant-disperseds that 0.1~5mL concentration is 0.01~1mol/L
Gold chloride；Wherein, the concentration of gold chloride is 0.1~0.5mmol/L in the gold chloride of the surfactant-dispersed.
3. the preparation method of electrum hollow polyhedral according to claim 1 or 2, it is characterised in that described goes back
Former agent is using at least one of citric acid, sodium citrate, potassium citrate, ascorbic acid, sodium ascorbate.
4. the preparation method of electrum hollow polyhedral according to claim 1 or 2, it is characterised in that it is described to
The gold chloride of reducing agent and surfactant-dispersed is sequentially added in the silver nanocubes of the surfactant-dispersed to be included：
Reducing agent is added into the silver nanocubes of the surfactant-dispersed while stirring, then stirs 2~10min, then add
Enter the gold chloride of surfactant-dispersed.
5. the preparation method of electrum hollow polyhedral according to claim 1 or 2, it is characterised in that the surface
The concentration of surfactant is 0.02~0.2mol/L in the silver nanocubes that activating agent disperses；The surfactant-dispersed
Gold chloride in the concentration of surfactant be 0.02~0.2mol/L.
6. the preparation method of electrum hollow polyhedral according to claim 1 or 2, it is characterised in that the table
Face activating agent is using polyvinylpyrrolidone, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, dodecyl
At least one of sodium sulphate, halogenated phosphates.
7. the preparation method of electrum hollow polyhedral according to claim 1 or 2, it is characterised in that pair
The solid obtained after centrifugation, which carries out washing, to be included：The solid obtained after centrifugation is washed using distilled water and absolute ethyl alcohol
Wash repeatedly.
8. the preparation method of electrum hollow polyhedral according to claim 1 or 2, it is characterised in that described adopts
Silver nanocubes are prepared with polyol reduction method in 150~195 DEG C of oil baths to comprise the following steps：
Step A1, be respectively configured by solvent of 1,5- pentanediols the silver nitrate solution, concentration that concentration is 10~50mg/mL be 10~
The polyvinylpyrrolidonesolution solution and concentration of 50mg/mL is the anhydrous cupric chloride solution of 10~50mg/mL, and by the anhydrous chlorine
Change copper solution to be distributed in the silver nitrate solution, so as to obtain the silver nitrate solution containing anhydrous cupric chloride；
Step A2,1,5-PD is taken in reaction vessel, and is placed in 150~195 DEG C of oil baths, with 200~300r/
The speed stirring of min, is allowed to thermally equivalent, keeps the temperature 10~30min, be then alternately added into the reaction vessel in step A1
Silver nitrate solution and polyvinylpyrrolidonesolution solution, the speed of addition be 50~200uL/min, the number of addition is 16~22
It is secondary；
Step A3, after adding completely, the reaction vessel is taken out, is cooled to room temperature while stirring, then the reaction is held
Solution in device is washed, so as to prepare silver nanocubes.
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| CN109056073A (en) * | 2018-07-19 | 2018-12-21 | 西安交通大学 | A kind of fast synthesis method of the ultra-fine electrum nano wire of hydrophilic and clean surface monocrystalline |
| CN109719305A (en) * | 2019-02-11 | 2019-05-07 | 石河子大学 | A kind of preparation method of the adjustable Au-Ag alloy nano particle of plasmon resonance |
| CN111347059A (en) * | 2020-03-30 | 2020-06-30 | 江南大学 | Synthesis method of porous gold @ silver @ gold nanocubes |
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| CN111347059A (en) * | 2020-03-30 | 2020-06-30 | 江南大学 | Synthesis method of porous gold @ silver @ gold nanocubes |
| CN111850528A (en) * | 2020-07-10 | 2020-10-30 | 南京大学 | Anti-oxidation and anti-vulcanization protection method for surface of nano silver wire |
| CN113231643A (en) * | 2021-05-06 | 2021-08-10 | 中南大学 | Biomedical noble metal frame material and preparation method and application thereof |
| CN114505487A (en) * | 2022-03-08 | 2022-05-17 | 南京邮电大学 | Preparation method of Au-Ag nano-framework |
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