CN105866098A - Cu2O-Au composite microparticle surface enhanced Raman scattering active substrate and production method thereof - Google Patents

Cu2O-Au composite microparticle surface enhanced Raman scattering active substrate and production method thereof Download PDF

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CN105866098A
CN105866098A CN201610227463.0A CN201610227463A CN105866098A CN 105866098 A CN105866098 A CN 105866098A CN 201610227463 A CN201610227463 A CN 201610227463A CN 105866098 A CN105866098 A CN 105866098A
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cu2o
micron
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enhanced raman
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CN105866098B (en
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张永军
陈雷
王雅新
赵月
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Jilin Normal University
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    • 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
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    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons

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Abstract

The invention provides a Cu2O-Au composite microstructure surface enhanced Raman scattering active substrate and a production method thereof. The method comprises the following steps: chelating citrate ions and copper ions, shaping with polyvinylpyrrolidone, and carrying out a reaction under water bath conditions with glucose as a reducing agent to generate Cu2O octahedral crystals; and dispersing the Cu2O octahedral crystals in water, adding a AuCl<4><-> solution, reducing AuCl<4><-> by the Cu2O octahedral crystals to form Au nanoparticles, and carrying out Au nanoparticle in situ deposition on the surface of octahedral Cu2O to reduce the surface energy of a system and generate Cu2O-Au composite microparticles. A Cu2O-Au composite microstructure is designed and synthesized to develop the surface enhanced Raman scattering activity of a semiconductor Cu2O, and local surface plasma resonance of Au aggregate and strong electromagnetic field generated in an interface due to charge transfer between Cu2O and Au are used to improve the surface enhanced Raman scattering activity of the Cu2O-Au composite microstructure.

Description

A kind of Cu2O-Au is combined micron particle surface-enhanced Raman scattering activity substrate and preparation method thereof
Technical field
The invention belongs to field of nanometer material technology.
Background technology
Surface enhanced Raman scattering effect is due to the absorption of the species such as molecule or very close to when having the surface of certain nanostructured, The phenomenon that its Raman signal is obviously enhanced than its body phase molecule.The generally accepted surface enhanced raman spectroscopy of people strengthens mechanism two Individual: Electromagnetic enhancement and Chemical enhancement.As a kind of surface spectrum, surface enhanced raman spectroscopy technology has high selectivity, height The advantages such as sensitivity, Non-Destructive Testing and adjustable point research, are widely used in Surface Science, chemistry and bio-sensing, biology The fields such as medical science detection and trace analysis detection.Quasiconductor Cu2O material is widely used in catalysis, sensing and solar energy The fields such as conversion.But, its weak surface-enhanced Raman scattering activity limits it in terms of surface enhanced raman spectroscopy field Application.
Summary of the invention
In order to improve quasiconductor Cu2The surface-enhanced Raman scattering activity of O, the present invention is by the side of Au nanoparticle growth in situ Method has been deposited on Cu2Octahedra Cu it has been prepared from O2O-Au is combined micron particle.
Wherein, Cu2The particle diameter of O is 1.4 μm；Cu2It is 1.2～1.6 μm that O-Au is combined the particle diameter of micron particle；Au nanoparticle Seed footpath is 17～28nm.
The octahedra Cu of preparation in the present invention2The method that O-Au is combined micron particle surface-enhanced Raman scattering activity substrate is specific as follows:
Step one, Cu2+React with mixed solution, generate copper citrate chelate.Described mixed solution is by soluble citrate Mix with hydrolysis inhibitor solution.Wherein, citrate is as chelating agen, optimization citric acid sodium or potassium citrate, Fructus Citri Limoniae The addition of hydrochlorate the most slightly excess, preferably excess 8%～9%.The preferred sodium carbonate of described hydrolysis inhibitor；
Step 2, add moulding dose of PVP K30 stirring and dissolving, polyvinylpyrrolidone and Cu2+Mol ratio More than 0.11；
Step 3, addition glucose, copper citrate is generated brick-red by glucose reduction under temperature is 70～90 DEG C of water bath condition Precipitation, scrubbed, be dried to obtain Cu2O octahedral crystal；
Step 4, by Cu2O octahedral crystal is dispersed in water, and adds AuCl4 -Cu after solution2O octahedral crystal surface Cu2O is by AuCl4 -The Au particle that reduction generates is deposited on octahedra Cu2The surface of O, generates Cu2O-Au micron is combined grain Son.Described AuCl4 -AuCl in solution4 -With Cu2The mol ratio of O is 8.90 × 10-2Below.
Bath temperature preferably 80 DEG C, Cu at such a temperature in the step 3 of the present invention2O has octahedral structure, too high or too low Temperature all will affect Cu2The pattern of O.
Beneficial effects of the present invention
1、Cu2On O surface, Au nanometer particle congery has the strongest localized surface plasmons resonance effect so that Cu2O-Au is combined micron particle and has good surface enhanced raman spectroscopy performance.
2, Au to Cu2The electric charge transfer of O so that there is the strongest electromagnetic field at its interface, also can further improve The surface enhanced raman spectroscopy performance of compound micron particle.
3, the Cu prepared2O crystal be shaped as octahedron, grain size narrow distribution, preparation process is controlled, react bar Part is gentle.
4, the Cu prepared2It is the best that O-Au is combined micron particle surface enhanced Raman scattering substrate pattern, Cu2On O surface The density of Au nanoparticle controlled, can be by regulation AuCl4 -Concentration to obtain surface enhanced raman spectroscopy performance best Compound micron particle.
5, the Cu prepared is made at the coefficient electromagnetic field of semiconductor-metal interface and chemical enhanced mechanism2O-Au is combined micro- The surface enhanced raman spectroscopy signal of rice structural system strengthens.
Accompanying drawing explanation
Fig. 1 is octahedra Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of O micro-crystal.
Fig. 2 is octahedra Cu in embodiment 1 in the present invention2The scanning electron microscope diagram of O micro-crystal.
Fig. 3 is octahedra 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 invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Fig. 5 is Cu in embodiment 1 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Fig. 6 is Cu in embodiment 1 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Fig. 7 is Cu in embodiment 2 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Fig. 8 is Cu in embodiment 2 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Fig. 9 is Cu in embodiment 2 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Figure 10 is Cu in embodiment 3 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Figure 11 is Cu in embodiment 3 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Figure 12 is Cu in embodiment 3 in the present invention2O-Au is combined the scanning electron microscope diagram of micrometer structure.
Figure 13 be in the present invention Au nanoparticle at octahedra Cu2The process schematic of growth on O micro-crystal.
During in Figure 14, (a) is the present invention 10-3M 4-MBA absorption is at octahedra Cu2The Raman collection of illustrative plates of O micro-crystal.(b,c, D) it is in the present invention 10-3M 4-MBA adsorbs at Cu2The SERS collection of illustrative plates of O-Au micron composite construction, the 1% of addition HAuCl4·4H2The volume of O solution is respectively: (b) 1.00mL, (c) 3.00mL and (d) 5.00mL.
Figure 15 is at Cu2O-Au is combined the balance of fermi level in micrometer structure (Ef) and causes electric charge to be transferred to Cu by Au2O Process schematic.
Figure 16 is Cu in embodiment 1 in the present invention2O-Au is combined the x-ray photoelectron power spectrum of Au 4f in micrometer structure.
Figure 17 is that SERS intensity is along with adding HAuCl4·4H2The increase of the volume of O solution and the graph of a relation that changes.Error bar Represent is the standard deviation of 5 different empirical values.
Detailed description of the invention
With the form of specific embodiment technical solution of the present invention it is further explained below and illustrates.
Reagent used in the embodiment of the present invention is as follows:
Copper sulphate pentahydrate (CuSO4·5H2O, traditional Chinese medicines chemical reagent company limited)
Two citric acid monohydrate trisodium (C6H5O7Na3·2H2O, traditional Chinese medicines chemical reagent company limited)
Natrium carbonicum calcinatum (Na2CO3, traditional Chinese medicines chemical reagent company limited)
Polyvinylpyrrolidone (PVP K30, traditional Chinese medicines chemical reagent company limited)
Glucose (C6H12O6·H2O, Beijing chemical reagent company limited)
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
First 0.68g CuSO is weighed4·5H2O、0.87g C6H5O7Na3·2H2O、0.51g Na2CO3、6.00g PVP K30、 1.11g C6H12O6·H2O and 3.00mL concentration is the HAuCl of 1%4·4H2O solution.
By CuSO4·5H2O is dissolved in 76mL deionized water.C6H5O7Na3·2H2O and Na2CO3It is dissolved in 4mL to go Ionized water is made sodium mixed solution.
Then, sodium mixed solution is added dropwise over the CuSO being stirred vigorously4·5H2In O solution, solution becomes navy blue.Dropping After end, above-mentioned mixed solution continues stirring 10 minutes, adds PVP in the solution being stirred vigorously.Solution is stirred vigorously 20 After minute, PVP is completely dissolved, and is added dropwise over the C of 4mL deionized water dissolving in solution6H12O6·H2O。
After completion of dropwise addition, being placed in by mixed solution in 80 DEG C of water-baths 15 minutes, solution becomes brick-red, then that solution is natural It is cooled to room temperature.By the solution centrifugal after above-mentioned cooling, clean, be placed in the vacuum drying oven of 60 DEG C and be dried 6 hours, Then octahedra Cu is obtained2O micron particle product.
By dried octahedra Cu2O micron particle is dissolved in 100mL deionized water.Then, to the Cu being stirred vigorously2O Solution is added dropwise over the 1%HAuCl of 3.00mL4·4H2O solution, continues after completion of dropwise addition to be stirred vigorously 2 at ambient temperature Minute.Solution becomes brownish black from brick-red, indicates Cu2The formation of O-Au micron composite construction.Product is centrifugal, cleaning, It is placed in the vacuum drying oven of 60 DEG C and is dried 6 hours.
If Fig. 1～Fig. 3 is octahedra Cu in the present invention2O micron particle scanning electron microscope diagram under different enlargement ratios, Can show that from figure its size is about 1.4 μm, surface unusual light.
As shown in Fig. 4～Fig. 6, at Cu2O-Au is combined in micron particle, Cu2O-Au is combined the rib length of micrometer structure and is about 1.2 Micron, Au diameter of nano particles is about 21nm.Substantial amounts of Au nanometer particle congery is had to generate, the covering of Au nanoparticle Area is very big, the most little Cu2O surface exposure.
Embodiment 2
The present embodiment is HAuCl with the difference of embodiment 14·4H2The concentration of O is 1%, and addition is 1.00mL.
As shown in Fig. 7～Fig. 9, at Cu2O-Au is combined in micrometer structure, Cu2O-Au is combined the rib length of micrometer structure and is about 1.3 μm, Au diameter of nano particles is about 17nm, and it is deposited on Cu uniformly2On the surface of O micro-crystal.
Embodiment 3
The present embodiment is HAuCl with the difference of embodiment 1 and 24·4H2The concentration of O is 1%, and addition 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, Cu2The surface of O is all received by Au Rice corpuscles covers, almost without exposed Cu2O surface.Cu2The rib length of O-Au nucleocapsid micrometer structure is about 1.6 μm, and Au receives The diameter of rice corpuscles is about 28nm.
In above-mentioned steps, copper ion (Cu2+) and C6H5O7Na3·2H2O and Na2CO3Reaction, wherein C6H5O7Na3·2H2O As chelating agen, and add a small amount of Na2CO3To suppress C6H5O7Na3·2H2The hydrolysis of O, generates copper citrate after reaction. Fructus Citri Limoniae Acid copper is reduced by glucose under 80 DEG C of water bath condition, generates Cu2O crystal.The PVP added in course of reaction serves Stabilizer and the effect of moulding dose, help to form octahedra Cu2O micro-crystal.Because AuCl4 -/ Au (0.99V) and Cu2+/Cu2The difference of the standard electrode EMF of O (0.203V) so that AuCl4 -The most just can be by Cu2O reduces, The Au nanoparticle generated has been deposited directly to octahedra Cu to reduce the surface energy of system2The surface of O, generates Cu2O-Au micron complex (as shown in figure 13).Octahedra Cu2The density of O upper Au nanoparticle can be by addition HAuCl4·4H2The amount of O regulates, and is finally obtained in that the Cu that surface enhanced raman spectroscopy performance is best2O-Au is combined micron knot Structure.
Compliance test result
With 4-MBA as probe molecule, respectively to octahedra Cu2O micro-crystal and Cu2O-Au is combined micrometer structure and carries out surface Strengthen the sign of Raman scattering performance.4-MBA solution dehydrated alcohol is prepared, and concentration is 10-3M.Sample is molten at 4-MBA Liquid soaks 4 hours.Centrifugal, dried, microscope slide is pressed into a thin slice and measures Raman spectrum.The Raman spectrum of sample The LabRAM ARAMIS copolymerization Jiao's micro-Raman spectroscopy using Horiba Jobin Yvon company of France is measured, excitation wavelength For 633nm, the power arriving sample stage is about 0.75mW.Laser is after 50 times of object lens microscopic systems focus on, and hot spot is straight Footpath size is 1 μm.The SERS spectra of 4-MBA is 30s, the result of 2 cumulative measurements.
In Figure 14, a curve is 10-3M 4-MBA absorption is at octahedra Cu2Raman collection of illustrative plates on O micro-crystal, at Cu2O is micro- The surface enhanced raman spectroscopy signal of 4-MBA is not observed on meter Jing Ti.B, c and d curve is 10-3M 4-MBA inhales It is attached to Cu2O-Au is combined the surface enhanced raman spectroscopy collection of illustrative plates of micrometer structure.With Cu2O micro-crystal is compared, at Cu2O-Au It is observed that the surface enhanced raman spectroscopy signal of significantly 4-MBA in compound micrometer structure, lay respectively at 846, 1013,1075,1145,1183 and 1584cm-1。Cu2O-Au is combined the surface enhanced raman spectroscopy signal of micrometer structure system Strengthen owing 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 electric charge is transferred to Cu from Au2O。 Electric charge transfer further can be confirmed by x-ray photoelectron power spectrum, as shown in figure 16, and Cu2O-Au is combined in micrometer structure The surface plasma of Au absorbs compared with Au powder (84.0eV), moves towards higher combination energy direction, and this is owing to electricity Lotus is transferred to Cu from Au2O.So, at Cu2At O-Au interface, Au is positively charged and Cu2O is electronegative, and Au receives Rice corpuscles and Cu2Strong interaction is there is between O micro-crystal.At Cu2O-Au is combined in micrometer structure, " focus " Generate relevant with the spacing between Au nanoparticle.Along with the HAuCl added4·4H2The increase of O volume, Au nanoparticle it Between spacing diminish, " focus " of generation becomes many, and surface plasmon resonance effect becomes strong, but, when adding HAuCl4·4H2O Volume when being 5.00mL, 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, almost without exposed Cu2O surface.At Cu2The Au nanoparticle meeting of excess on O surface Hide most Cu2The surface-enhanced Raman scattering activity point at O-Au interface so that surface enhanced raman spectroscopy signal reduces.
As shown in figure 17, surface enhanced raman spectroscopy signal is along with the HAuCl added4·4H2The increase of the volume of O, presents First strengthen (1.00～3.00mL) and reduce the trend of (3.00～5.00mL) afterwards.

Claims (9)

1. a Cu2O-Au is combined micron particle, it is characterised in that its structure is that Au nanoparticle is deposited on octahedron Cu2O micron particle surface and formed.
Cu the most according to claim 12O-Au is combined micron particle, it is characterised in that Cu2The particle diameter of O is 1.4 micro- Rice.
Cu the most according to claim 12O-Au is combined micron particle, it is characterised in that Cu2O-Au is combined micron grain The particle diameter of son is about 1.2-1.6 micron.
Cu the most according to claim 12O-Au is combined micron particle, it is characterised in that Au nano particle diameter is about 17-28 nanometer.
5. the Cu described in a claim 12O-Au is combined the preparation method of micron particle, specifically comprises the following steps that
Step one, Cu2+React with the mixed solution of soluble citrate and hydrolysis inhibitor, generate copper citrate chelate； Described citrate is that excess adds；
Step 2, add moulding dose of PVP K30 stirring and dissolving, polyvinylpyrrolidone and Cu2+Mol ratio More than 0.11；
Step 3, addition glucose, copper citrate is generated brick-red by glucose reduction under temperature is 70～90 DEG C of water bath condition Precipitation, scrubbed, be dried to obtain Cu2O octahedral crystal；
Step 4, by Cu2O octahedral crystal is dispersed in water, and adds AuCl4 -Cu after solution2O octahedral crystal surface Cu2O is by AuCl4 -The Au particle that reduction generates is deposited on octahedra Cu2The surface of O, generates Cu2O-Au micron is combined grain Son；Described AuCl4 -AuCl in solution4 -With Cu2The mol ratio of O is 8.90 × 10-2Below.
Cu the most according to claim 52O-Au is combined the preparation method of micron particle, it is characterised in that solubility lemon Lemon hydrochlorate is sodium citrate or potassium citrate.
Cu the most according to claim 52O-Au is combined the preparation method of micron particle, it is characterised in that solubility lemon Lemon hydrochlorate excess 8%～9%.
Cu the most according to claim 52O-Au is combined the preparation method of micron particle, it is characterised in that described water Solution inhibitor is sodium carbonate.
9. the Cu described in a claim 12O-Au is combined micron particle and is 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
CN107315044A (en) * 2017-06-16 2017-11-03 重庆医科大学 Based on octahedra 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
CN109095492A (en) * 2018-08-29 2018-12-28 淮阴师范学院 The preparation method of octahedra uniform morphology cuprous oxide micron crystalline substance
CN109342400A (en) * 2018-12-06 2019-02-15 中国科学院苏州纳米技术与纳米仿生研究所 Application of the semiconducting compound in the identification and identification in grape wine source area
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
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
CN114684848A (en) * 2022-04-25 2022-07-01 延安大学 Cu2Preparation method of O nanometer quadrangular bipyramid

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李文鹏: "贵金属Au及其核壳结构纳米粒子的制备与SERS性能研究", 《中国优秀硕士学位论文全文数据库》 *
杨宇婷，张洁，刘宗健，吕德义: "聚乙烯吡咯烷酮与柠檬酸钠的加入量对葡萄糖还原法制备Cu2O颗粒形貌的影响", 《青岛科技大学学报（自然科学版）》 *
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN107315044A (en) * 2017-06-16 2017-11-03 重庆医科大学 Based on octahedra 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
CN109095492A (en) * 2018-08-29 2018-12-28 淮阴师范学院 The preparation method of octahedra uniform morphology cuprous oxide micron crystalline substance
CN109342400A (en) * 2018-12-06 2019-02-15 中国科学院苏州纳米技术与纳米仿生研究所 Application of the semiconducting compound in the identification and identification in grape wine source area
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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