CN108333168A - A kind of enhancing Raman detection method using satellite structure - Google Patents
A kind of enhancing Raman detection method using satellite structure Download PDFInfo
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- CN108333168A CN108333168A CN201810403280.9A CN201810403280A CN108333168A CN 108333168 A CN108333168 A CN 108333168A CN 201810403280 A CN201810403280 A CN 201810403280A CN 108333168 A CN108333168 A CN 108333168A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
A kind of enhancing Raman detection method using satellite structure is related to Raman spectrum.1) gold, silver nano-particle is synthesized；2) extremely thin and dense oxide shell layer is coated in the gold, silver nanoparticle surface of step 1) synthesis；3) nano material to be measured is modified, is then assembled in the nanoparticle surface that step 2) obtains, form Jin Weihe, oxide is shell, and nano material is the composite material of satellite, abbreviation SHINERS satellite structures；4) composite material that step 3) obtains is placed in the environment containing testing molecule, so that testing molecule is adsorbed on composite material surface, and tested using Raman spectrometer, to obtain the Raman signal of testing molecule.Solve the problems, such as that traditional SERS technologies are difficult to be used in the nano material for being widely used in the fields such as catalytic science, environmental science, energy science.
Description
Technical field
The present invention relates to Raman spectrums, more particularly, to a kind of profit for enhancing Raman signal on transition-metals and their oxides
With the enhancing Raman detection method of satellite structure.
Background technology
Raman spectrum is a kind of fingerprint vibrational spectrum technology, can be used for specific recognition and the detection of substance.However, traditional
Raman spectrum have the shortcomings that sensitive DEG C it is low.This just significantly limits the application of Raman spectrum.The last century 70's,
The Raman signal that the discoveries such as Van Duyne are adsorbed on the molecule of gold, silver nano-material surface can be enhanced to million times or more.This
One effect gradually develops into a new technology --- Surface enhanced Raman spectroscopy (SERS).
SERS has high surface sensitive DEG C, its general enhancement factor is up to 106~1012, under optimal conditions very
To up to the Single Molecule Detection limit.Meanwhile it also has many advantages, such as water resistant interference, the detection in suitable lower wave number region.Therefore, table
Face enhancing Raman spectrum has broad application prospects in fields such as electrochemistry, analysis science, life sciences.However, long-term
Research shows that only gold, silver, Tong Deng coin race metal just have stronger Raman enhancing activity；And for other materials (such as mistake
Cross metal and its oxide etc.), Raman enhancing activity is very low, or even does not have Raman enhancing ability (material limitation).Separately
On the one hand, even gold, silver, Tong Deng coin race metal material, also require them that there is specific nanoscale rough surface (often
Tens nanometers to hundreds of nanometers), just there is SERS effects, therefore SERS be also not used to be now widely used for catalytic science,
The nano material (its size is generally all in 10nm or less) (pattern limitation) in the fields such as environmental science, energy science.Material and shape
Limitation in looks has greatly affected the application of SERS.Therefore researcher has been devoted to expand the universality of SERS.
One of the solution of SERS Problem of Universality is the development of " borrowing power " strategy.The discoveries such as Weaver pass through electrochemistry
Method the surface of coarse gold, silver electrode or nano-particle deposit one layer of transition metal SERS can be expanded to platinum, palladium,
The transition metal such as ruthenium, rhodium.(Sungho Park,Pengxiang Yang,Piedad Corredor,Michael
J.Weaver.Transition Metal-Coated Nanoparticle Films:Vibrational
Characterization with Surface-Enhanced Raman Scattering.J.Am.Chem.Soc.2002,
124,2428-2429.) this method is referred to as " borrowing power " by they.Its principle is generated using kernel gold, silver nano-particle
Extremely strong local Electromagnetic enhancement is adsorbed on the Raman signal of the transiting metal surfaces molecule such as outer layer platinum, palladium.Using by means of power strategy,
They obtain the Raman signal that CO is adsorbed on the transition metal such as platinum, palladium, ruthenium, rhodium, and have studied them under electrochemical conditions
Changing rule.The applicant has further developed the strategy of " borrowing power ", using chemical synthesis in gold, silver nanoparticle surface
One layer of extremely thin and dense transition metal shell is directly coated, and shell thickness is adjustable, significantly simplifies " borrowing power " strategy
Operating procedure, and expanded its application range.(Jian-Feng Li,Zhi-Lin Yang,Bin Ren,Guo-Kun Liu,
Ping-Ping Fang,Yu-Xiong Jiang,De-Yin Wu,Zhong-Qun Tian.Surface-enhanced Raman
spectroscopy using gold-core platinum-shell nanoparticle film electrodes:
Toward a versatile vibrational strategy for electrochemical
Interfaces.Langmuir 2006,22,10372-10379) " borrowing power " tactful material for solving SERS in certain journey DEG C
Expect pervasive problem so that SERS can be expanded to transition metal material.However, being difficult that each material is equal in actual application
Controllably it is deposited on the surface of gold and silver.Simultaneously as be in direct contact between outer layer transition metal and kernel gold, silver nano material, and
There are apparent electronic action, the property so as to cause outer layer transition metal changes, therefore the Raman signal obtained also will
It is affected.On the other hand, the pattern Problem of Universality of its still unresolved SERS, that is, utilize " borrowing power " strategy still can not be in nanometer
Material (size<10nm) or smooth surface obtains Raman signal.
In order to solve the Problem of Universality of SERS, applicants have invented shell isolated nano particles to enhance Raman light within 2010
Spectrum, abbreviation SHINERS.(Chinese invention patent ZL201010044867.9 discloses a kind of enhanced with shell isolated nano particles and draws
The method of graceful spectrum；Jian Feng Li,Yi Fan Huang,Yong Ding,Zhi Lin Yang,Song Bo Li,Xiao
Shun Zhou,Feng Ru Fan,Wei Zhang,Zhi You Zhou,De Yin Wu,Bin Ren,Zhong Lin
Wang,Zhong Qun Tian.Shell-isolated nanoparticle-enhanced Raman
Spectroscopy.Nature 2010,464,392-395) in SHINERS, it is put using core A u nano-particles as signal
Big device enhances the Raman signal of molecule nearby.Simultaneously in one layer of extremely thin and dense SiO of Au outer claddings2Shell, formed shell every
Exhausted nano-particle completely cuts off the interaction between sample to be tested and Au, excludes the interference of other signals, to obtain sample to be tested certainly
The signal of body.SHINERS overcomes material and the pattern limitation of traditional SERS well, is theoretically utilized in any material peace
Sliding surface.For example, applicant obtains the Raman signal of single-crystal surface adsorbent using SHINERS, to realize monocrystalline
The on-spot study of surface reaction process.However, since SHINERS particle surfaces are inert SiO2Shell, can not binding molecule,
Therefore it is difficult the Raman detection for being directly used in specific molecular.It would therefore be highly desirable to develop it is a kind of can be applied to molecular specificity detection
Raman method.
Invention content
A kind of the object of the present invention is to provide universalities wide, sensitive DEG C of height, in gas, liquid trace materials it is quick
A kind of enhancing Raman detection method using satellite structure of analysis and detection.
The present invention includes the following steps：
1) gold, silver nano-particle is synthesized；
2) extremely thin and dense oxide shell layer is coated in the gold, silver nanoparticle surface of step 1) synthesis；
3) nano material to be measured is modified, is then assembled in the nanoparticle surface that step 2) obtains, forming gold is
Core, oxide are shell, and nano material is the composite material of satellite, abbreviation SHINERS satellite structures；
4) composite material that step 3) obtains is placed in the environment containing testing molecule, so that testing molecule is adsorbed on compound
Material surface, and tested using Raman spectrometer, to obtain the Raman signal of testing molecule.
In step 1), the size of the gold, silver nano-particle can be 30~200nm.
In step 2), the extremely thin and dense oxide shell layer can be selected from silica, aluminium oxide, titanium oxide, oxidation
The thickness of one kind in manganese etc., extremely thin and dense oxide shell layer can be 0.5~10nm；.
In step 3), the nano material to be measured can be selected from transition metal, transition metal alloy, transition metal oxide
One kind in；Electrostatic Absorption can be used in the mode that nano material to be measured is assembled in gold, silver nanoparticle surface or chemical bond is even
Connection etc.；The mode of the Electrostatic Absorption can be by nanomaterial assembly in gold-oxide core core/shell nanoparticles or silver-oxide core shell
Nano-particle, specific steps can be：
(1) gold-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles are utilized into ascorbic acid or citric acid
Sodium etc. is modified, and negative electricity on gold-oxide core core/shell nanoparticles or silver-oxide core shell nanoparticle surface band is made；
(2) nano material to be measured is modified using cetyl trimethylammonium bromide or nitrous tetrafluoroborate etc.,
Nano-material surface to be measured is set to become positively charged；
(3) step (1) and (2) resulting materials are placed in water, ethyl alcohol, acetonitrile, n,N-Dimethylformamide equal solvent
One kind vibrating at least 12h, makes nanomaterial assembly in the surface of core-shell nano.
It is described by chemical bond coupling in the way of can be by nanomaterial assembly in gold-oxide core core/shell nanoparticles or silver-
Oxide core core/shell nanoparticles, specific steps can be：
It (1) can sulfydryl silicon using amino silane by gold-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles
The coupling agents such as alkane are modified；
(2) by the gold after modification-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles and nanometer material to be measured
Material is placed in one kind in water, ethyl alcohol, acetonitrile, n,N-Dimethylformamide equal solvent, vibrates at least 12h, makes nanomaterial assembly
In the surface of core-shell nano.
The present invention synthesizes the gold or Nano silver grain of certain size first, and extremely thin and dense oxide is coated on its surface
Then oxide shell layer surface is modified and be assembled in nano material to be measured by shell, formed by gold-oxide-nanometer material
Core-shell structure copolymer-satellite structure the compound for expecting composition is used in combination it to remove absorption test substance.Finally will utilize laser Raman spectrometer into
Row test can obtain the Raman signal of test substance.
Beneficial effects of the present invention are as follows：
It is difficult to be widely used in catalytic science, environment section that the method disclosed in the present, which solves traditional SERS technologies,
The problem of being used in the nano material (its size is generally all in 10nm or less) in the fields such as, energy science.Compared to existing skill
Art, the present invention possessed by advantage it is as follows：
(1) traditional SERS substrates are using naked Au, Ag as reinforcing material, therefore very weak to very polymolecular absorption, therefore very
Hardly possible realizes their detection.The present invention is defended by assembling specific satellite structure outside shell isolated nano particles by regulation and control
The material of star structure, can specificity absorption testing molecule, to realize its detection；
(2) the method disclosed in the present can be by the composition material of change satellite structure, to realize different molecular
Detection has good versatility, and easy to operate；
(3) by that in gold (or silver) one layer of extremely thin and dense oxide shell layer of nano-particle outer cladding, can completely cut off point
Son is adsorbed on kernel gold (or silver) nanoparticle surface, can also exclude the electronics between nano material and gold (or silver) nano-particle
Effect, to make the Raman signal true and accurate of acquisition；Shell can also improve the stability of particle simultaneously so that it can be applied to
At more exacting terms (such as high temperature, strong acid etc.)；
(4) by the coupling between satellite structure and shell isolated nano particles, sensitive DEG C of detection can be improved, and can
It is directly used in the detection of substance in solution.
Description of the drawings
Fig. 1 is nanomaterial assembly on gold (or silver) oxide core core/shell nanoparticles (SHINERS satellite structures) surface
Illustraton of model.
Fig. 2 is that nano platinum particle is assembled in Au@SiO2The scanning electron microscope and transmission electron microscope picture on nucleocapsid surface.
Fig. 3 is that nano platinum particle is assembled in Au@SiO2The transmission electron microscope picture on nucleocapsid surface.
Fig. 4 is the Raman figure detected using SHINERS satellite structures in solution to sulfydryl nitrobenzene.In Fig. 4, curve a
For Au@SiO2@Pt satellite structures, curve b are Pt nano-particles.
Fig. 5 is the Raman figure that isocyanobenzene, cinnamic acid in solution are detected using SHINERS satellite structures.In Figure 5, curve a
For Pd- isocyanobenzenes, curve b is Pt- cinnamic acids.
Fig. 6 is the scanning electron microscope (SEM) photograph that gold nanoparticle is assembled in golden@oxide core shells nanoparticle surface.
Fig. 7 is the Raman spectrogram that 4-Mercaptopyridine in solution is detected using SHINERS satellite structures.In the figure 7, curve
A is shell isolated nano particles satellite structure；Curve b is shell isolated nano particles.
Fig. 8 is the Raman figure using CO in SHINERS satellite structure detection gas.
Fig. 9 is the Raman figure using ethylene in SHINERS satellite structure detection gas.
Specific implementation mode
Following embodiment will the invention will be further described in conjunction with attached drawing.
Embodiment 1
Au@SiO2The synthesis of core-shell nano：
Take 100mL 0.01%HAuCl4, after heating is boiled, under at the uniform velocity stirring condition, rapidly join 1.4mL's 1%
Trisodium citrate aqueous solution after keeping boiling 30min, stops reacting and being cooled to room temperature to get being about 55nm to average grain diameter
Aurosol.The freshly prepared aurosols of the 30mL are taken, are placed in round-bottomed flask, the amino silane of 0.4mL 1mmol/L is added
Solution, and it is vigorously stirred 15min.The sodium silicate aqueous solution that dense DEG C of 3.2mL is 0.54% is added, continues after stirring 10min, adds
Heat keeps 30min to 90 DEG C.Then stop reaction, SiO can be made by being cooled to room temperature2The Au@SiO of shell thickness about 2nm2
Core-shell nano.
Embodiment 2
Nano platinum particle is assembled in Au@SiO2Core-shell nano surface：
1mL nano platinum particle colloidal sols to be measured (size about 3nm) are taken, 1mL NOBF are added4Solution, after acutely shaking 30min,
It centrifuges.Supernatant is removed, obtained solid is scattered in 1mL water.Above-mentioned dispersion liquid 0.1mL is taken, the fresh preparations of 1mL are added
Au@SiO2In core-shell nano colloidal sol, 10h or more is stirred.It is then centrifuged for detaching, obtained solid is Au@SiO2@Pt satellites
Structure, model (provide nano material, oxide shell layer and gold (or silver) nano-particle to be measured) respectively as shown in Figure 1.Fig. 2,
Fig. 3 is respectively the characterization result of scanning electron microscope and transmission electron microscope.By Fig. 2 and 3 it is found that nano platinum particle can be equal by this method
It is assembled in Au@SiO evenly2Core-shell nano surface, obtained material abbreviation SHINERS satellite structures.
Embodiment 3
Molecules in solution is detected using SHINERS satellite structures：
By method shown in embodiment 2, Au@SiO are prepared2@Pt or Au@SiO2@Pd satellite structures.Take the above-mentioned satellite knots of 50 μ L
Structure drops on silicon chip.After natural drying, 10min is impregnated in solution such as sulfydryl nitrobenzene, isocyanobenzene or cinnamic acids, then
Directly carry out Raman test.Nano platinum particle to be measured is directly taken to be soaked in 10min in sulfydryl nitrobenzene solution, then simultaneously
Raman test is carried out to make reference.
Fig. 4 is respectively to be adsorbed on Au@SiO to sulfydryl nitrobenzene2Raman test knot on@Pt and common nano platinum particle
Fruit.As seen from the figure, for common nano platinum particle, enhance ability since it does not have Raman, so not observing when test
Any Raman signal.And for Au@SiO2@Pt satellite structures, since Au nano-particles can enhance the molecule being adsorbed on Pt
Raman signal, it is possible to the apparent Raman signal observed to sulfydryl nitrobenzene.Wherein Raman shift is in 1340cm-1Place
Spectral peak can belong to the eigen vibration of nitro, 1530cm-1The spectral peak at place can be attributed to the eigen vibration of phenyl ring.This is similarly used
Kind satellite structure, successfully realizes the Raman detection of isocyanobenzene in solution, cinnamic acid, the results are shown in Figure 5.
Embodiment 4
Nano-particle is assembled in Au@SiO2Core-shell nano surface：
Take 100mL 0.01%HAuCl4, after heating is boiled, under at the uniform velocity stirring condition, rapidly join 1~6mL's 1%
Trisodium citrate aqueous solution after keeping boiling 30min, stops reacting and being cooled to room temperature to get being about 30nm to average grain diameter
Aurosol.It can refer to a kind of Chinese patent CN201710803044.1 (conjunctions of very thin shell isolated big grain size gold nanoparticle
At method), but 200 μ L 1mmol mercaptopyridines (MPY) are first added before sodium metasilicate is added, synthesis is coated with MPY molecules
Obtained SHINS is carried out amination processing by the Au SHINs of 120nm：20ml Au SHINs colloidal sols, are slowly added to acidifying solution
It is centrifuged after 4ml (40ml water, 1ml 0.1mol HCl, 400 μ L amino silane solution are uniformly mixed) 20min, takes supernatant away, add
Enter 20ml 30nm Au colloidal sols.It is uniformly mixed, 4 DEG C stand overnight, you can gold nanoparticle is assembled into SHINs particle surfaces,
The results are shown in Figure 6.Obtained satellite structure is centrifuged, carries out Raman test, and by the SHINs of itself and unassembled satellite
Raman signal compared, the results are shown in Figure 7.
Embodiment 5
Utilize molecule in SHINERS satellite structure detection gas：
By method shown in embodiment 2, Au@SiO are prepared2@Pt or Au@SiO2@Pd satellite structures.Take the above-mentioned satellite knots of 50 μ L
Structure drops on silicon chip.After natural drying, 10min is placed in the atmosphere containing 1%CO or 1% ethylene, then directly carries out Raman
Test.
Fig. 8 is respectively to utilize Au@SiO2@Pt or Au@SiO2The Raman test knot of CO in@Pd satellite structure detection gas
Fruit.Since Au nano-particles can enhance the Raman signal for the molecule being adsorbed on Pt or Pd, it is possible to obviously observe CO
Raman signal.Au@SiO2486cm then can be observed on@Pt satellite structures-1And 2096cm-1Two Raman peaks.They could divide
It is not attributed to the stretching vibration of the Pt-C keys and C=O keys of wire type CO absorption.Similarly, Au@SiO are utilized2@Pd satellite structures pair
Ethylene in gas is detected, and also can obviously observe the Raman signal (Fig. 9) of ethylene.
Claims (8)
1. a kind of enhancing Raman detection method using satellite structure, it is characterised in that include the following steps：
1) gold, silver nano-particle is synthesized；
2) in the oxide coated shell of gold, silver nanoparticle surface of step 1) synthesis；
3) nano material to be measured is modified, is then assembled in the nanoparticle surface that step 2) obtains, form Jin Weihe, oxygen
Compound is shell, and nano material is the composite material of satellite, abbreviation SHINERS satellite structures；
4) composite material that step 3) obtains is placed in the environment containing testing molecule, testing molecule is made to be adsorbed on composite material
Surface, and tested using Raman spectrometer, to obtain the Raman signal of testing molecule.
2. a kind of enhancing Raman detection method using satellite structure as described in claim 1, it is characterised in that in step 1),
The size of the gold, silver nano-particle is 30~200nm.
3. a kind of enhancing Raman detection method using satellite structure as described in claim 1, it is characterised in that in step 2),
The one kind of the oxide shell layer in silica, aluminium oxide, titanium oxide, manganese oxide.
4. a kind of enhancing Raman detection method using satellite structure as described in claim 1 or 3, it is characterised in that in step 2)
In, the thickness of the oxide shell layer is 0.5~10nm.
5. a kind of enhancing Raman detection method using satellite structure as described in claim 1, it is characterised in that in step 3),
The one kind of the nano material to be measured in transition metal, transition metal alloy, transition metal oxide.
6. a kind of enhancing Raman detection method using satellite structure as described in claim 1, it is characterised in that in step 3),
The mode that the nano material to be measured is assembled in gold, silver nanoparticle surface is coupled using Electrostatic Absorption or chemical bond.
7. a kind of enhancing Raman detection method using satellite structure as claimed in claim 6, it is characterised in that the electrostatic is inhaled
Attached mode is by nanomaterial assembly in gold-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles, specific step
Suddenly it is：
(1) by gold-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles using ascorbic acid or sodium citrate into
Row modification, makes negative electricity on gold-oxide core core/shell nanoparticles or silver-oxide core shell nanoparticle surface band；
(2) nano material to be measured is modified using cetyl trimethylammonium bromide or nitrous tetrafluoroborate, is made to be measured
Nano-material surface becomes positively charged；
(3) step (1) and (2) resulting materials are placed in one kind in water, ethyl alcohol, acetonitrile, n,N-Dimethylformamide equal solvent,
At least 12h is vibrated, makes nanomaterial assembly in the surface of core-shell nano.
8. a kind of enhancing Raman detection method using satellite structure as claimed in claim 6, it is characterised in that the utilizationization
The mode for learning key coupling is by nanomaterial assembly in gold-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles,
The specific steps are：
It (1) can hydrosulphonyl silane etc. using amino silane by gold-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles
Coupling agent is modified；
(2) gold after modification-oxide core core/shell nanoparticles or silver-oxide core core/shell nanoparticles are set with nano material to be measured
One kind in Yu Shui, ethyl alcohol, acetonitrile, n,N-Dimethylformamide solvent vibrating at least 12h, makes nanomaterial assembly in nucleocapsid
The surface of nano-particle.
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| PCT/CN2018/101544 WO2019205364A1 (en) | 2018-04-28 | 2018-08-21 | Enhanced raman detection method using satellite structure |
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| WO2019205364A1 (en) * | 2018-04-28 | 2019-10-31 | 厦门斯贝克科技有限责任公司 | Enhanced raman detection method using satellite structure |
| CN110687100A (en) * | 2019-11-26 | 2020-01-14 | 启东科赛尔纳米科技有限公司 | Core-shell type nanoparticle with high SERS (surface enhanced Raman scattering) enhanced activity and SERS quantitative detection substrate |
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| CN109358033B (en) * | 2019-01-08 | 2019-04-30 | 中国科学院烟台海岸带研究所 | One seed nucleus-satellite type gold and silver composite Nano SERS substrate and preparation method thereof |
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