CN109596822A - A kind of gold core silver shell nanocomposite and preparation method thereof - Google Patents
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Abstract
The present invention relates to a kind of golden core silver shell nanocomposite and its preparations, the composite material includes the gold nano grain of bicone and is wrapped in outside gold nano grain in rodlike silver nano-grain, and the mass ratio of the gold nano grain and silver nano-grain is (0.8~1): (0.77~3.75).Compared with prior art, it is directly to grow rodlike silver nanoparticle shell in the monodispersed and cuspidated Au NBPs nano material of tool that the present invention, which synthesizes Au NBP Ag NRs shell core nano material, it ensures that the nanocomposite of synthesis has good monodispersity and adjustable draw ratio, increases the application range of this nanocomposite.
Description
Technical field
The present invention relates to Raman detection technical fields, and in particular to a kind of gold core silver shell nanocomposite and its preparation side
Method.
Background technique
Raman spectrum is that nineteen twenty-eight India physicist Raman is removed in discovery scattering spectrum when studying the scattering spectrum of benzene
There is there is also very weak and frequency is different with incident light spectrum except Rayleigh Scattering Spectra identical from incident light spectrum frequency
Inelastic scattering spectrum.This inelastic scattering spectrum is known as Raman scattering.The raman scattering spectrum of molecule is substantially right
Answer energy difference between the molecular energy level.Therefore, the Raman scattering of molecule can be used to identify the structure of molecule.Raman also because
His discovery and the Nobel Prize in physics for obtaining nineteen thirty.Since Raman spectrum is not influenced by water in sample, with laser
Appearance and laser detector technology progress, Raman spectrum obtains in fields such as environmental contaminants, medicine, biology and macromolecules
To being widely applied, have many advantages, such as intuitive, rapid, accurate, lossless.But since Raman spectrum itself is very weak, scattering
The intensity of signal only has the 10 of incident light6~107/ mono-, the application of Raman spectrum is greatly limited, for example, Raman
Spectrum is difficult to realize the detection and analysis of low concentrations of molecular.Therefore people develop one kind can be realized Raman scattering intensities improve it is several
Enhancing Raman scattering method, that is, Surface enhanced Raman scattering (SERS) of a order of magnitude, that has expanded Raman scattering significantly applies model
It encloses.
Surface enhanced Raman scattering phenomenon is that Fleishmann in 1974 is seen in coarse silver electrode surface from pyridine for the first time
It measures, later, the presence of SERS is demonstrated by a series of experimental and theoretical computation by Van and his partner.SERS
The form of expression be mainly some Molecular Adsorptions to when metallic plasma nano material (also referred to as SERS substrate) performance, molecule
Raman scattering signal can be greatly improved.When especially these metal nano materials are gold, silver and bronze, the width of signal enhancing
It spends bigger.Therefore, SERS substrate is to generate the key factor of SERS, is that Surface enhanced Raman spectroscopy technology is applied to every field
Basis.SERS substrate performance directly affects the application of Surface enhanced Raman spectroscopy technology.In general, good SERS substrate
Good with enhancing performance, performance structure is uniform, and preparation facilitates the features such as waiting.
The nano particle of the gold, silver and bronze especially nano particle of gold and silver has very strong Raman reinforcing effect, therefore, often
SERS substrate is the nano particle of gold and silver.But the nano material of pure gold or silver has serious material diversity
Limitation, the price of gold nano-material is high, and silver nano material more vivaciously prepares more difficult to control and table due to chemical property
Face is oxidized easily or vulcanizes and forms insulating layer Raman active is caused to reduce, moreover, silver nano-grain bio-toxicity is higher.Separately
Outside, for current gold, silver nano particle generally in spherical, SERS activity can not obtain good promotion.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of biocompatibility number,
Enhance the good golden core silver shell nanocomposite and preparation method thereof of performance.
The purpose of the present invention can be achieved through the following technical solutions: a kind of gold core silver shell nanocomposite, this is multiple
Condensation material includes the gold nano grain of bicone and is wrapped in outside gold nano grain in rodlike silver nano-grain, the gold
The mass ratio of nano particle and silver nano-grain is (0.8~1): (0.77~3.75).
This gold and silver core-shell nano composite material combines that gold nano-material physical and chemical stability is good and bio-toxicity is low
The advantages of while combine the advantage of silver nano material better Raman enhancing activity.This is because the chemistry of gold nano grain
Nature comparison is than relatively inert and reason that the silver nano-grain chemical property rate of exchange are active.Furthermore diconical golden core and rodlike
Silver-colored shell increases the asymmetry of composite material, and the both ends of this asymmetry, that is, stick can increase the density of electron cloud, into one
Step increases the Raman active of composite material.It is this that the characteristics of increasing Raman active is caused to be referred to as " lightning-arrest due to asymmetry
Needle effect ".
A kind of preparation method of golden core silver shell nanocomposite as described above, comprising the following steps:
(1) gold chloride and trisodium citrate are mixed, and sodium borohydride is added under intense agitation, be vigorously stirred mixed
It closes uniformly to be placed in oil bath and be reacted, be centrifugated, be cooled to room temperature after reaction, obtain Au seed；
(2) gold chloride, silver nitrate and hydrochloric acid are sequentially added under intense agitation to cetyl trimethyl bromination
In ammonium salt solution, ascorbic acid is then added, adds the Au seed that step (1) is prepared, is transferred in water-bath and reacts, to anti-
It is centrifugated after answering, and ultrasonic disperse will be precipitated into water, obtain Au NBPs；
(3) the Au NBPs that step (2) obtains is added under intense agitation molten to cetyl trimethylammonium bromide
Then liquid sequentially adds ascorbic acid, silver nitrate and sodium hydroxide, is vigorously stirred, be then centrifuged for separation, clean to get described
Golden core silver shell nanocomposite.
Preferably, the stirring rate being vigorously stirred described in step (1)~(3) is 400~1200rpm, is vigorously stirred
It is carried out under the conditions of 25~35 DEG C, being vigorously stirred is in order to which the substance for allowing reaction to generate can be uniformly dispersed in the solution moment.
Preferably, gold chloride described in step (1), trisodium citrate, sodium borohydride molar ratio be (2~5): (40~
80): (5~12.5).
Preferably, the temperature of oil bath described in step (1) is 70~85 DEG C, and the oil bath time is 1~4h, and due to process
In, the rate of stirring is 120~300rpm.
Preferably, the gold chloride, silver nitrate, hydrochloric acid, ascorbic acid of addition and the molar ratio of Au seed are in step (2)
(500~3000): (100~600): (20000~120000): (800~4800): (2~45).
Preferably, the temperature of water-bath described in step (2) is 25~35 DEG C, and water bath time is 1~2.5h.
Preferably, the molar ratio of Au NBPs, ascorbic acid, silver nitrate and the sodium hydroxide that are added in step (3) be (1~
1.5): (25~35): (2~5): (30~60).
Preferably, ascorbic acid, silver nitrate and sodium hydroxide are added to cetyl trimethylammonium bromide in step (3)
After solution, it is vigorously stirred 5~30min.
Preferably, the revolving speed of centrifuge separation described in step (1)~(3) is 6000~10000r/min, revolving speed centrifugation
Condition further aspect can be good at nano material to separate from solution, on the other hand can guarantee that material will not be because of centrifugation
Revolving speed is excessively high and reunites.
Compared with prior art, the beneficial effects of the present invention are embodied in following several respects:
(1) synthetic method quickly time saving and environmental protection and energy saving.
(2) synthesis shell core nano material is directly to grow in the monodispersed and cuspidated Au NBPs nano material of tool
Rodlike silver nanoparticle shell out, it is ensured that the nanocomposite of synthesis has good monodispersity and adjustable draw ratio,
Increase the application range of this nanocomposite.
(3) shell core nano material of the present invention combine the biocompatibility of gold nano-material, physical and chemical stability and
The SERS activity of silver nano material.
(4) the Au NBP@Ag NRs shell core nanocomposite energy with very strong SERS activity and monodispersity synthesized
It is enough further to synthesize the highly sensitive Raman microprobe with cancer cell targeting, for the detection and imaging of tumour cell,
The treatment of cancer and context of detection play a significant role.
Detailed description of the invention
Fig. 1 is the uv absorption spectra for the Au seed that embodiment 1 is prepared；
The TEM figure that Fig. 2 is the Au NBPs that embodiment 1 is prepared；
Fig. 3 is the uv absorption spectra for the Au NBPs that embodiment 1 is prepared；
Fig. 4 is the TEM figure for the composite material that embodiment 1 is prepared；
Fig. 5 is the Raman spectrum for the composite material that embodiment 1 is prepared.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
In the present invention, all chemical reagent used are that analysis is pure or more, and without any processing.Chlorine gold
Acid (HAuCl4·4H2O) and ascorbic acid (L-ascorbic Acid) purchase is in the smooth Science and Technology Ltd. of upper Haitai, cetyl
Ammonium bromide (CTAB), cetyl chloride ammonium (CTAC) are bought in Aladdin Co., Ltd.Hydrochloric acid (HCl, 37%), sodium borohydride
(NaBH4), silver nitrate (AgNO3) and trisodium citrate (Na3Ct) purchase is in traditional Chinese medicines Co., Ltd.Deionization used in experiment
Water is prepared in real time by Millipore-Q ultrapure water system (Millipore company, the U.S.), and conductivity is not less than 18.2M Ω
cm-1。
(1) preparation of Au nanometers of seeds
Firstly, under conditions of 30 DEG C of magnetic agitations, the 5 of 0.5 milliliterMM every literChlorauric acid solution, 5 milliliters
0.1 mole of every liter of cetyl chloride ammonium and the 0.1 of 0.5 milliliter mole of trisodium citrate mix a stir evenly.Later in play
Freshly prepd 0.25 milliliter ice-cold of 25 mMs every liter of sodium borohydride solution is added under conditions of strong stirring, is vigorously stirred
2 minutes.The color of reaction solution becomes dark brown by glassy yellow.Then above-mentioned solution is being placed into 80 DEG C of oil bath pan
Gentle agitation 4 hours, the color of solution gradually became bright-coloured claret by dark brown.Obtain claret Au seed solution from
After being removed in oil bath pan, cools down under room temperature, obtain the Au seed solution of form stable.Compared to the Au kind reported before
Son, we synthesize Au seed normal temperature condition under can save for a long time.Obtained Au seed is subjected to ultraviolet spectra detection, is obtained
Result as shown in Figure 1, from the figure we can see that, Au seed has apparent ultraviolet absorption peak at 520nm.
(2) preparation of Au NBPs
Using CTAB as template, Au seeds is nucleus, and Au seeds is containing gold chloride, CTAB, hydrochloric acid and anti-ization hematic acid
Growth-promoting media in can be grown to gold nano bipyramid (Au NBPs), wherein gold chloride is as precursors, hydrochloric acid conditioning solution
PH value controls reaction rate, and ascorbic acid is as mild reducing agent.Specific synthesis step are as follows: 30 DEG C of conditions being vigorously stirred
Under, 0.5 milliliter of 10 mMs every liter of chlorauric acid solution, 100 microlitres of 10 mMs every liter of silver nitrate solution and 200 micro-
1 mole every liter of the hydrochloric acid risen is added sequentially in the CTAB solution containing 0.1 mole every liter of 10 milliliters, is vigorously stirred, is obtained
To bright yellow solution, it is added 80 microlitres of 0.1 mole every liter of ascorbic acid, solution becomes colorless clear solution at once, obtains
Growth-promoting media is added immediately the Au seeds solution of certain volume (60~300 microlitres), is vigorously stirred 10min, and obtained solution moves
Except it is glitch-free in 30 DEG C of water-bath after stirrer under the conditions of continue to keep 2h.Solution is in 9500 turns of 10 minutes conditions
Lower centrifugation is washed with deionized once, and precipitating is re-dispersed into 5 milliliters of deionized water, and ultrasonic disperse obtains Au
NBPs.Obtained Au NBPs is subjected to TEM detection, as a result as shown in Fig. 2, therefrom we can see that obtained Au NBPs is non-
Chang Junyi.Meanwhile obtained Au NBPs is subjected to ultraviolet spectra detection, obtained result is as shown in figure 3, we can from figure
To find out, by adjusting the volume for the Au seeds being added, longitudinal plasma absorption peak of Au NBPs can be regulated and controled.
(3) preparation of Au NBP@Ag NRs shell core nano material
Based on Au NBPs, we synthesize the gold of golden bipyramid core Silver nanorod shell using a kind of method of novel quickly green
Galactic nucleus shell nanocomposite (Au NBP@Ag NRs).Under 30 DEG C of intense agitations, 1.2 milliliters of above-mentioned Au NBPs is being stirred
It is added under conditions of mixing in 6 milliliters of 0.04 mole every liter of CTAB solution.Then sequentially add 0.1 mole of 156 microlitres
Every liter of ascorbic acid solution, the 10 of 250 microlitres mMs of every liter of silver nitrate solutions and the 0.1 of 348 microlitres mole every liter
Sodium hydroxide solution, be vigorously stirred 10min, be centrifuged ten minutes under conditions of 8000 rpms, remove supernatant, spend from
Sub- water centrifuge washing, solution is re-dispersed into ultrasonic disperse in 4 milliliters of deionized water, and to obtain Au NBP@Ag NRs gel molten
Liquid.Above-mentioned Au NBP@Ag NRs gel solution is subjected to TEM test, as a result as shown in figure 4, showing the core-shell nano material of synthesis
Material has good monodispersity.
(4) the active assessment of the SERS of Au NBP@Ag NRs and the identification of low concentration small-molecule substance
In order to assess the SERS activity of Au NBP@Ag NRs, we are respectively 5 microlitres of Au NBPs solution and Au NBP@
Ag NRs solution is added dropwise on the smooth copper sheet of two panels, dry under the conditions of gravity-flow ventilation, obtains Au NBPs and Au NBP@
The SERS substrate of Ag NRs.Meanwhile we select a kind of small molecule solution (10 of low concentration-6M R6G) as detection substance, divide
The 10 of 1 microlitre are not taken-6The R6G solution of M is added dropwise in SERS substrate, detects the enhanced drawing of SERS substrate using Raman spectrometer
Graceful signal.Fig. 5 is shown, in the case where low-power and quickly detection (30mW, 1s), Au NBPs and Au NBP@Ag NRs
SERS substrate can be able to detect that the SERS signal of R6G in the R6G solution of low concentration, it will be apparent that Au NBP@Ag
NRs SERS substrate has stronger signal strength, and it is better to illustrate that Au NBP@Ag NRs shell core nanocomposite has
SERS activity can be used in the small-molecule substance with Raman signal for detecting low concentration.
Embodiment 2
Using preparation method similar to Example 1, the difference is that:
(1) micromolar containing 2 micromoles (μm ol) gold chloride and 40 micromole's trisodium citrates and 1000 by 20 milliliters
CTAC mixing, and 5 micromole's sodium borohydrides are added while stirring under the conditions of 25 DEG C, 400rpm, continue stirring and is allowed to mixing
It is even, it is subsequently placed in 70 DEG C of oil baths and is reacted, be centrifugated, be cooled to room temperature after 4h, obtain 2 micromolar Au seeds；
(2) by the solution of 5 micromole's gold chlorides, 1 micromole's silver nitrate and 200 micromole's hydrochloric acid in 25 DEG C, 400rpm item
It is sequentially added under part into 0.1 mole every liter of 10 milliliters of cetyl trimethylammonium bromide solution, 8 micromoles is then added
Ascorbic acid adds 0.02 micromole's Au seed that step (1) is prepared, is transferred in 25 DEG C of water-baths and reacts, after 2.5h
Centrifuge separation, and ultrasonic disperse will be precipitated into water, it obtains 5 milliliters and contains 5 micromolar Au NBPs；
(3) Au NBPs obtained in 1 micromolar step (2) is taken out and is added under the conditions of 25 DEG C, 400rpm to ten
Six alkyl trimethyl ammonium bromide solution, then sequentially add ascorbic acid, silver nitrate and sodium hydroxide, wherein Au NBPs, resist
The molar ratio of bad hematic acid, silver nitrate and sodium hydroxide is that 1:25:5:30 continues to stir, and is then centrifuged for separation, cleans to get described
Golden core silver shell nanocomposite.
Through detecting, the golden core silver shell nanocomposite which is prepared has better SERS activity, can
For detecting the small-molecule substance with Raman signal of low concentration.
Embodiment 3
Using preparation method similar to Example 1, the difference is that:
(1) contain 5 micromole's gold chlorides, 80 micromole's trisodium citrates mixing and 1000 micromolar 16 for 20 milliliters
12.5 micromolar sodium borohydrides are added in the solution of alkyl trimethyl ammonium chloride while stirring under the conditions of 35 DEG C, 1200rpm, after
Continuous stirring is allowed to uniformly mixed, is subsequently placed in 85 DEG C of oil baths and is reacted, is centrifugated, is cooled to room temperature after 1h, it is micro- to obtain 5
Mole Au seed；
(2) by the mixed solution containing 30 micromolar gold chlorides, 6 micromole's silver nitrates and 120 micromole's hydrochloric acid 35
DEG C, the cetyl trimethylammonium bromide solution that 10 milliliters of concentration is 0.1 mole every liter is added sequentially under the conditions of 1200rpm
In, 48 micromolar ascorbic acid are then added, adds 0.45 micromole's Au seed that step (1) is prepared, is transferred to
It reacts in 35 DEG C of water-baths, is centrifugated after 1h, and ultrasonic disperse will be precipitated into water, obtain Au NBPs；
(3) the Au NBPs for obtaining step (2) is added under the conditions of 35 DEG C, 1200rpm to cetyl trimethyl bromination
Then ammonium salt solution sequentially adds ascorbic acid, silver nitrate and sodium hydroxide, wherein Au NBPs, ascorbic acid, silver nitrate and hydrogen
The molar ratio of sodium oxide molybdena is that 1.5:35:2:60 continues to stir, and is then centrifuged for separation, cleans and answer to get the golden core silver shell nanometer
Condensation material.
Through detecting, the golden core silver shell nanocomposite which is prepared has better SERS activity, can
For detecting the small-molecule substance with Raman signal of low concentration.
Claims (10)
1. a kind of gold core silver shell nanocomposite, which is characterized in that the composite material include the gold nano grain of bicone with
And be wrapped in outside gold nano grain in rodlike silver nano-grain, the mass ratio of the gold nano grain and silver nano-grain is
(0.8~1): (0.77~3.75).
2. a kind of preparation method of golden core silver shell nanocomposite as described in claim 1, which is characterized in that including following step
It is rapid:
(1) gold chloride and trisodium citrate are mixed, and sodium borohydride is added under intense agitation, it is equal to be vigorously stirred mixing
Even be placed in oil bath is reacted, and is centrifugated, is cooled to room temperature after reaction, and Au seed is obtained；
(2) gold chloride, silver nitrate and hydrochloric acid are sequentially added under intense agitation molten to cetyl trimethylammonium bromide
In liquid, ascorbic acid is then added, adds the Au seed that step (1) is prepared, is transferred in water-bath and reacts, wait react knot
It is centrifugated after beam, and ultrasonic disperse will be precipitated into water, obtain Au NBPs；
(3) the Au NBPs that step (2) obtains is added under intense agitation to cetyl trimethylammonium bromide solution,
Then ascorbic acid, silver nitrate and sodium hydroxide are sequentially added, is vigorously stirred, separation is then centrifuged for, cleans to get the golden core
Silver-colored shell nanocomposite.
3. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
(1) stirring rate being vigorously stirred described in~(3) be 400~1200rpm, be vigorously stirred under the conditions of 25~35 DEG C into
Row.
4. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
(1) gold chloride described in, trisodium citrate, sodium borohydride molar ratio be (2~5): (100~200): (5~12.5).
5. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
(1) temperature of oil bath described in is 70~85 DEG C, and the oil bath time is 1~4h, and since in the process, the rate of stirring is 120
~300rpm.
6. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
(2) molar ratio of the gold chloride, silver nitrate, hydrochloric acid, ascorbic acid and the Au seed that are added in is (500~3000): (100~
600): (20000~120000): (800~4800): (2~45).
7. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
(2) temperature of water-bath described in is 25~35 DEG C, and water bath time is 1~2.5h.
8. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
(3) molar ratio of Au NBPs, ascorbic acid, silver nitrate and the sodium hydroxide that are added in is (1~1.5): (25~35): (2~
5): (30~60).
9. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
(3) ascorbic acid, silver nitrate and sodium hydroxide are added to cetyl trimethylammonium bromide solution in, it is vigorously stirred 5~
30min。
10. a kind of preparation method for stating golden core silver shell nanocomposite according to claim 2, which is characterized in that step
Suddenly the revolving speed of centrifuge separation described in (1)~(3) is 6000~10000r/min.
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| CN112692298A (en) * | 2020-12-01 | 2021-04-23 | 中国人民解放军战略支援部队航天工程大学 | Preparation method of core-shell structure nano gold and silver composite material substrate |
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| CN110739358A (en) * | 2019-09-25 | 2020-01-31 | 江苏大学 | gold-lead sulfide core-shell nanorod photodetectors and preparation method thereof |
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| CN112285088A (en) * | 2020-09-23 | 2021-01-29 | 嘉兴学院 | Microgel serving as surface enhanced Raman scattering substrate and preparation method and application thereof |
| CN112692298A (en) * | 2020-12-01 | 2021-04-23 | 中国人民解放军战略支援部队航天工程大学 | Preparation method of core-shell structure nano gold and silver composite material substrate |
| CN112828283A (en) * | 2020-12-31 | 2021-05-25 | 纳米籽有限公司 | High-purity gold nanoparticles, selectively-coated gold nanoparticles and preparation method thereof |
| CN114047173A (en) * | 2021-11-05 | 2022-02-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Surface-enhanced Raman spectrum substrate and preparation method and application thereof |
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