CN105866098B - A kind of Cu2Compound micro particles surface-enhanced Raman scattering activity substrate of O-Au and preparation method thereof - Google Patents
A kind of Cu2Compound micro particles surface-enhanced Raman scattering activity substrate of O-Au and preparation method thereof Download PDFInfo
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- CN105866098B CN105866098B CN201610227463.0A CN201610227463A CN105866098B CN 105866098 B CN105866098 B CN 105866098B CN 201610227463 A CN201610227463 A CN 201610227463A CN 105866098 B CN105866098 B CN 105866098B
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- 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
The present invention provides a kind of Cu2Compound micrometer structure surface-enhanced Raman scattering activity substrate of O-Au and preparation method thereof.By citrate ion and chelating copper ions, polyvinylpyrrolidone moulding is recycled, generates Cu under water bath condition using glucose as reducing agent2O octahedral crystal.By Cu2O octahedral crystal is dispersed in water, and AuCl is added4 ‑After solution, Cu2O octahedral crystal is by AuCl4 ‑Reduction generates Au nanoparticle, and in order to reduce the surface energy of system, Au nanoparticle in-situ deposition is in octahedra Cu2The surface of O, generates Cu2The compound micro particles of O-Au.In order to expand semiconductor Cu2The surface-enhanced Raman scattering activity of O, the present invention have designed and synthesized Cu2The compound micrometer structure of O-Au utilizes the localized surface plasmons resonance and Cu of Au aggregation2Electric charge transfer between O and Au and in the strong-electromagnetic field that interface generates, improve the Cu of synthesis2The surface-enhanced Raman scattering activity of the compound micrometer structure of O-Au.
Description
Technical field
The invention belongs to field of nanometer material technology.
Background technique
Surface enhanced Raman scattering effect is due to the absorption of the species such as molecule or very close to certain nanostructure
When surface, the phenomenon that Raman signal is significantly increased than its body phase molecule.The generally accepted Surface enhanced Raman scattering of people increases
There are two strong mechanism: Electromagnetic enhancement and Chemical enhancement.As a kind of surface spectrum, Surface enhanced Raman scattering technology has height
The advantages such as selectivity, highly sensitive, non-destructive testing and adjustable point research, are widely used in Surface Science, chemistry and biology
The fields such as sensing, biomedical detection and trace analysis detection.Semiconductor Cu2O material is widely used in catalysis, sensing
With solar energy conversion etc. fields.But weak surface-enhanced Raman scattering activity limits it in Surface enhanced Raman scattering
Application in terms of field.
Summary of the invention
In order to improve semiconductor Cu2The surface-enhanced Raman scattering activity of O, the present invention is by Au nanoparticle growth in situ
Method be deposited on Cu2Octahedra Cu has been prepared on O2The compound micro particles of O-Au.
Wherein, Cu2The partial size of O is 1.4 μm;Cu2The partial size of the compound micro particles of O-Au is 1.2~1.6 μm;Au nanoparticle
Seed diameter is 17~28nm.
Octahedron Cu is prepared in the present invention2The method of the compound micro particles surface-enhanced Raman scattering activity substrate of O-Au has
Body is as follows:
Step 1: Cu2+It is reacted with mixed solution, generates copper citrate chelate.The mixed solution is by soluble lemon
Hydrochlorate and hydrolysis inhibitor solution mix.Wherein, citrate is as chelating agent, optimization citric acid sodium or potassium citrate,
The additional amount of citrate is usually slightly excessive, and preferably excessive 8%~9%.The preferred sodium carbonate of the hydrolysis inhibitor;
Step 2: moulding agent PVP K30 and stirring and dissolving, polyvinylpyrrolidone and Cu is added2+Rub
You are than being greater than 0.11;
Step 3: glucose is added, copper citrate is restored by glucose in the case where temperature is 70~90 DEG C of water bath conditions and is generated
Brick-red precipitating, it is washed, be dried to obtain Cu2O octahedral crystal;
Step 4: by Cu2O octahedral crystal is dispersed in water, and AuCl is added4 -Cu after solution2O octahedral crystal surface
Cu2O is by AuCl4 -The Au particle deposition generated is restored in octahedra Cu2The surface of O, generates Cu2O-Au microns of compound particles.Institute
State AuCl4 -AuCl in solution4 -With Cu2The molar ratio of O is 8.90 × 10-2Below.
Preferably 80 DEG C of bath temperature in step three of the invention, at such a temperature Cu2O have octahedral structure, it is excessively high or
Too low temperature all will affect Cu2The pattern of O.
Beneficial effects of the present invention
1、Cu2Au nanometer particle congery has very strong localized surface plasmons resonance effect on the surface O, so that
Cu2The compound micro particles of O-Au have good Surface enhanced Raman scattering performance.
2, Au to Cu2The electric charge transfer of O also can be mentioned further so that there is very strong electromagnetic fields at its interface
The Surface enhanced Raman scattering performance of high compound micro particles.
3, the Cu prepared2The shape of O crystal is octahedron, and particle size narrow distribution, preparation process is controllable, reaction
Mild condition.
4, the Cu prepared2The compound micro particles surface enhanced Raman scattering substrate pattern of O-Au is very good, Cu2The surface O
On Au nanoparticle density it is controllable, can pass through adjust AuCl4 -Concentration obtain Surface enhanced Raman scattering performance most
Good compound micro particles.
5, make the Cu prepared in the coefficient electromagnetic field of semiconductor-metal interface and chemical enhanced mechanism2O-Au
The Surface enhanced Raman scattering signal enhancing of compound micrometer structure system.
Detailed description of the invention
Fig. 1 is octahedron Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of O micro-crystal.
Fig. 2 is octahedron Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of O micro-crystal.
Fig. 3 is octahedron Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of O micro-crystal.
Fig. 4 is Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Fig. 5 is Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Fig. 6 is Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Fig. 7 is Cu in embodiment 2 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Fig. 8 is Cu in embodiment 2 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Fig. 9 is Cu in embodiment 2 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Figure 10 is Cu in embodiment 3 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Figure 11 is Cu in embodiment 3 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Figure 12 is Cu in embodiment 3 in the present invention2The scanning electron microscope diagram of the compound micrometer structure of O-Au.
Figure 13 be in the present invention Au nanoparticle in octahedra Cu2The process schematic grown on O micro-crystal.
(a) is 10 in the present invention in Figure 14-3M 4-MBA is adsorbed on octahedra Cu2The Raman map of O micro-crystal.(b,c,
It d) is 10 in the present invention-3M 4-MBA is adsorbed on Cu2The SERS map of O-Au microns of composite constructions, 1% HAuCl of addition4·
4H2The volume of O solution is respectively: (b) 1.00mL, (c) 3.00mL and (d) 5.00mL.
Figure 15 is in Cu2The balance of fermi level (Ef) in the compound micrometer structure of O-Au and cause charge to be transferred to by Au
Cu2The process schematic of O.
Figure 16 is Cu in embodiment 1 in the present invention2The x-ray photoelectron spectroscopy of Au 4f in the compound micrometer structure of O-Au.
Figure 17 is SERS intensity with addition HAuCl4·4H2The increase of the volume of O solution and the relational graph changed.Error
What stick represented is the standard deviation of 5 different empirical values.
Specific embodiment
Technical solution of the present invention is further explained and is illustrated in the form of specific embodiment below.
Reagent used in the embodiment of the present invention is as follows:
Cupric sulfate pentahydrate (CuSO4·5H2O, traditional Chinese medicines chemical reagent Co., Ltd)
Two citric acid monohydrate trisodiums (C6H5O7Na3·2H2O, traditional Chinese medicines chemical reagent Co., Ltd)
Natrium carbonicum calcinatum (Na2CO3, traditional Chinese medicines chemical reagent Co., Ltd)
Polyvinylpyrrolidone (PVP K30, traditional Chinese medicines chemical reagent Co., Ltd)
Glucose (C6H12O6·H2O, Beijing chemical reagent Co., Ltd)
Tetra chlorauric acid (HAuCl4·4H2O, Shanghai Si Yu Chemical Industry Science Co., Ltd)
4- mercaptobenzoic acid (4-MBA, Sigma-Aldrich trade Co., Ltd)
Embodiment 1
0.68g CuSO is weighed first4·5H2O、0.87g C6H5O7Na3·2H2O、0.51g Na2CO3、6.00g PVP
K30、 1.11g C6H12O6·H2The HAuCl that O and 3.00mL concentration is 1%4·4H2O solution.
By CuSO4·5H2O is dissolved in 76mL deionized water.C6H5O7Na3·2H2O and Na2CO3It is dissolved in 4mL deionization
Sodium mixed solution is made in water.
Then, sodium mixed solution is added dropwise to the CuSO being vigorously stirred4·5H2In O solution, solution becomes navy blue.Drop
After adding, above-mentioned mixed solution continues stirring 10 minutes, and PVP is added into the solution being vigorously stirred.Solution is vigorously stirred 20
After minute, PVP is completely dissolved, and the C with 4mL deionized water dissolving is added dropwise into solution6H12O6·H2O。
After completion of dropwise addition, mixed solution is placed in 80 DEG C of water-baths 15 minutes, solution becomes brick-red, then certainly by solution
So it is cooled to room temperature.Above-mentioned solution after cooling is centrifuged, cleaning, is placed in 60 DEG C of vacuum oven dry 6 hours,
Then octahedra Cu is obtained2O micron particles product.
By the octahedra Cu after drying2O micron particles are dissolved in 100mL deionized water.Then, to being vigorously stirred
Cu2The 1%HAuCl of 3.00mL is added dropwise in O solution4·4H2O solution continues at room temperature acutely after completion of dropwise addition
Stirring 2 minutes.Solution becomes brownish black from brick-red, shows Cu2The formation of O-Au microns of composite constructions.Product is centrifuged, is clear
It washes, is placed in 60 DEG C of vacuum oven dry 6 hours.
If FIG. 1 to FIG. 3 is octahedron Cu in the present invention2Scanning electron microscopy of the O micro particles under different enlargement ratios
Mirror figure, for Cong Tuzhong it can be concluded that its particle size is about 1.4 μm, surface is very smooth.
As shown in Fig. 4~Fig. 6, in Cu2In the compound micro particles of O-Au, Cu2The rib length of the compound micrometer structure of O-Au is about
1.2 microns, Au diameter of nano particles is about 21nm.There is a large amount of Au nanometer particle congery to generate, the covering of Au nanoparticle
Area is very big, only seldom Cu2O surface exposure.
Embodiment 2
The present embodiment is difference from example 1 is that HAuCl4·4H2The concentration of O is 1%, additional amount 1.00mL.
As shown in fig. 7~fig. 9, in Cu2In the compound micrometer structure of O-Au, Cu2The rib length of the compound micrometer structure of O-Au is about
1.3 μm, Au diameter of nano particles is about 17nm, is uniformly deposited on Cu2On the surface of O micro-crystal.
Embodiment 3
The present embodiment and Examples 1 and 2 are the difference is that HAuCl4·4H2The concentration of O is 1%, and additional amount is
5.00mL。
Structural characterization
As shown in Figure 10~Figure 12, the structure of formation is Cu2O-Au core-shell structure copolymer micrometer structure, Cu2It is all received by Au on the surface of O
Rice corpuscles covering, almost without exposed Cu2The surface O.Cu2The rib of O-Au nucleocapsid micrometer structure is about 1.6 μm long, Au nanoparticle
The diameter of son is about 28nm.
In above-mentioned steps, copper ion (Cu2+) and C6H5O7Na3·2H2O and Na2CO3It reacts, wherein C6H5O7Na3·2H2O
As chelating agent, and a small amount of Na is added2CO3To inhibit C6H5O7Na3·2H2The hydrolysis of O generates copper citrate lemon after reaction
Sour copper is restored under 80 DEG C of water bath conditions by glucose, generates Cu2O crystal.The PVP being added during the reaction plays stabilization
The effect of agent and moulding agent, help form octahedra Cu2O micro-crystal.Because of AuCl4 -/ Au (0.99V) and Cu2+/Cu2O
The difference of the standard electrode EMF of (0.203V), so that AuCl4 -It at room temperature can be by Cu2O reduction, the Au nanometer of generation
Particle has been deposited directly to octahedra Cu to reduce the surface energy of system2The surface of O, generates Cu2O-Au microns compound
Object (as shown in figure 13).Octahedra Cu2The density of the upper Au nanoparticle of O can pass through the HAuCl of addition4·4H2The amount of O is adjusted
Section, can finally obtain the best Cu of Surface enhanced Raman scattering performance2The compound micrometer structure of O-Au.
Compliance test result
Using 4-MBA as probe molecule, respectively to octahedra Cu2O micro-crystal and Cu2The compound micrometer structure of O-Au carries out table
The characterization of face enhancing Raman scattering performance.4-MBA solution is prepared with dehydrated alcohol, concentration 10-3M.Sample is in 4-MBA solution
Impregnate 4 hours.After centrifugation, drying, thin slice measurement Raman spectrum is pressed on glass slide.The Raman spectrum of sample uses method
The LabRAM ARAMIS of Horiba Jobin Yvon company, state is copolymerized burnt micro-Raman spectroscopy measurement, and excitation wavelength is
633nm, the power for reaching sample stage is about 0.75mW.Laser is after 50 times of object lens microscopic systems focus, spot diameter size
It is 1 μm.The SERS spectra of 4-MBA is the result of 30s, 2 cumulative measurements.
A curve is 10 in Figure 14-3M 4-MBA is adsorbed on octahedra Cu2Raman map on O micro-crystal, in Cu2O is micro-
The Surface enhanced Raman scattering signal of 4-MBA is not observed on meter Jing Ti.B, c and d curve are 10-3M 4-MBA is adsorbed on
Cu2The Surface enhanced Raman scattering map of the compound micrometer structure of O-Au.With Cu2O micro-crystal is compared, in Cu2O-Au is compound micro-
It can be observed that the Surface enhanced Raman scattering signal of apparent 4-MBA, is located at 846,1013,1075 in rice structure,
1145,1183 and 1584cm-1。Cu2The enhancing of the Surface enhanced Raman scattering signal of the compound micrometer structure system of O-Au is attributed to
In the coefficient electromagnetic field of semiconductor-metal interface and chemical enhanced mechanism.
As shown in figure 15, Au and Cu2The fermi level of O is respectively 0.45V and 0.47V, and charge is transferred to Cu from Au2O.Electricity
Lotus shifts and can further be confirmed by x-ray photoelectron spectroscopy, as shown in figure 16, Cu2Au in the compound micrometer structure of O-Au
Surface plasma absorbs compared with Au powder (84.0eV), and mobile towards higher combination energy direction, this is attributed to charge from Au
It is transferred to Cu2O.So, in Cu2At O-Au interface, Au is positively charged and Cu2O is negatively charged, Au nanoparticle and Cu2O is micro-
There is strong interactions between meter Jing Ti.In Cu2In the compound micrometer structure of O-Au, the generation of " hot spot " and Au nanoparticle
Between spacing it is related.With the HAuCl of addition4·4H2The increase of O volume, the spacing between Au nanoparticle become smaller, and generate
" hot spot " become more, surface plasmon resonance effect becomes strong, still, as addition HAuCl4·4H2The volume of O is 5.00mL
When, as shown in Figure 10~12, generate Cu2O-Au core-shell structure copolymer micrometer structure, Cu2The surface of O is all covered by Au nanoparticle, several
Not exposed Cu2The surface O.In Cu2Excessive Au nanoparticle can cover most of Cu on the surface O2The table at the interface O-Au
Face enhances Raman scattering active point, so that Surface enhanced Raman scattering signal reduces.
As shown in figure 17, Surface enhanced Raman scattering signal with addition HAuCl4·4H2The increase of the volume of O is presented
First enhancing (1.00~3.00mL) reduces the trend of (3.00~5.00mL) afterwards out.
Claims (4)
1. a kind of Cu2The compound micro particles of O-Au, which is characterized in that its structure is that Au nanoparticle is deposited on octahedra Cu2O
Micro particles surface and formed;Cu2The partial size of O is 1.4 microns;Cu2The partial size of the compound micro particles of O-Au is about 1.2-1.6 micro-
Rice;Au nano particle diameter is about 17-28 nanometers.
2. a kind of Cu described in claim 12The preparation method of the compound micro particles of O-Au, the specific steps are as follows:
Step 1: Cu2+It is reacted with the mixed solution of soluble citrate and hydrolysis inhibitor, generates copper citrate chelate;
The citrate is excessive is added;Soluble citrate excessive 8% ~ 9%;The hydrolysis inhibitor is sodium carbonate;
Step 2: moulding agent PVP K30 and stirring and dissolving, polyvinylpyrrolidone and Cu is added2+Molar ratio
Greater than 0.11;
Step 3: glucose is added, copper citrate is restored by glucose in the case where temperature is 70 ~ 90 DEG C of water bath conditions and generates brick red
Color precipitating, it is washed, be dried to obtain Cu2O octahedral crystal;
Step 4: by Cu2O octahedral crystal is dispersed in water, and AuCl is added4 -Cu after solution2The Cu on O octahedral crystal surface2O
By AuCl4 -The Au particle deposition generated is restored in octahedra Cu2The surface of O, generates Cu2O-Au microns of compound particles;It is described
AuCl4 -AuCl in solution4 -With Cu2The molar ratio of O is 8.90 × 10-2Below.
3. Cu according to claim 22The preparation method of the compound micro particles of O-Au, which is characterized in that soluble citric acid
Salt is sodium citrate or potassium citrate.
4. a kind of Cu described in claim 12The compound micro particles of O-Au are used as surface-enhanced Raman scattering activity substrate.
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CN106323940A (en) * | 2016-08-24 | 2017-01-11 | 合肥学院 | Method for in situ monitoring visible photocatalysis and organic dye degradation based on superficially reinforced Raman spectra technology |
CN107315044B (en) * | 2017-06-16 | 2020-04-28 | 重庆医科大学 | Based on octahedron Cu2O-Au electrochemical aptamer sensor and preparation method thereof |
CN108459003A (en) * | 2018-01-17 | 2018-08-28 | 安徽农业大学 | A kind of preparation method of silver nano-grain coating zinc oxide surface enhanced Raman scattering effect substrate |
CN110116008A (en) * | 2018-02-07 | 2019-08-13 | 中国科学院兰州化学物理研究所苏州研究院 | The regulatable Au-Cu in interface2O photochemical catalyst and preparation method thereof |
CN109095492B (en) * | 2018-08-29 | 2020-08-11 | 淮阴师范学院 | Preparation method of octahedral cuprous oxide micron crystal with uniform morphology |
CN109342400B (en) * | 2018-12-06 | 2021-06-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Application of semiconductor compound in identification and identification of origin of wine |
CN109675584A (en) * | 2019-01-11 | 2019-04-26 | 山东师范大学 | A kind of semiconductor material Cu2The preparation method and application of O@Au |
CN114684848A (en) * | 2022-04-25 | 2022-07-01 | 延安大学 | Cu2Preparation method of O nanometer quadrangular bipyramid |
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