CN113308685B - Silver nano/foam copper material and preparation method and application thereof - Google Patents

Silver nano/foam copper material and preparation method and application thereof Download PDF

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CN113308685B
CN113308685B CN202110569767.6A CN202110569767A CN113308685B CN 113308685 B CN113308685 B CN 113308685B CN 202110569767 A CN202110569767 A CN 202110569767A CN 113308685 B CN113308685 B CN 113308685B
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foam
silver nano
copper
foam copper
copper sheet
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CN113308685A (en
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张德
李琛
吴卓群
余志�
梁培
倪德江
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Jiangxi Sericulture Tea Research Institute (jiangxi Economic Crop Research Institute)
Huazhong Agricultural University
China Jiliang University
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Jiangxi Sericulture Tea Research Institute (jiangxi Economic Crop Research Institute)
Huazhong Agricultural University
China Jiliang University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/54—Contact plating, i.e. electroless electrochemical plating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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

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Abstract

The invention discloses a preparation method of an SERS substrate made of silver nano/foamy copper materials. The SERS substrate made of the silver nano/copper foam material is low in material cost, simple in preparation method, high in stability, storage-resistant and high in sensitivity in Raman detection.

Description

Silver nano/foam copper material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of surface-enhanced Raman scattering spectroscopy, and particularly relates to a silver nano/foam copper material and a preparation method and application thereof.
Background
The copper foam is a novel multifunctional material with a large number of communicated or non-communicated holes uniformly distributed in a copper matrix, has good conductivity and ductility, and has lower preparation cost and better conductivity compared with the similar material nickel foam, so the copper foam is commonly used for preparing battery cathode (carrier) materials, catalyst carriers and electromagnetic shielding materials.
Surface Enhanced Raman Spectroscopy (SERS) is a technique for increasing the intensity of raman spectra by adsorbing molecules to be detected with noble metals and using an enhanced electric field on the metal surface. Because of its high sensitivity and quick detection, it has been widely used in many fields such as chemistry, bio-pharmaceuticals, medical detection and food safety. The enhancement mechanisms of SERS, which are currently generally accepted by academia, mainly include electromagnetic field Enhancement Mechanism (EM) and charge transfer enhancement mechanism (CT). The electromagnetic field Enhancement Mechanism (EM) considers that when light is incident to the surface of the SERS substrate, the nano structure on the surface of the substrate is excited to generate a local surface plasmon resonance phenomenon, so that a Raman signal of a molecule to be detected is greatly enhanced; another charge transfer enhancement mechanism (CT) is considered that when the metal surface is irradiated by light, the molecules to be detected adsorbed on the metal surface and the metal are transferred mutually by electrons to generate a resonance-like raman scattering phenomenon, so as to enhance the raman signal of the molecules to be detected.
The traditional SERS substrate material mainly includes a metal material, a semiconductor material, a metal/semiconductor composite material, and the like. The surface plasmon resonance of the noble metal silver can efficiently and rapidly enhance the regional electromagnetic field on the metal surface, and can adsorb more molecules to be detected under the nano structure, so that the method is often used for detecting the Surface Enhanced Raman Spectroscopy (SERS). For example, chinese patent document CN112630151A proposes a silver sol SERS substrate suitable for organophosphorus and carbamate sulfur-containing pesticide molecules, which reduces the lower limit of raman detection; however, the pure silver nanoparticles are not excellent enough in terms of molecular adsorption and hot spot number to be detected, and the enhancement effect needs to be further improved. As Chinese patent document CN108893714B specifically proposes an SERS substrate densely covered with Ag nano-columnar structures, the number of 'hot spots' of the substrate is increased through the nano-columnar structures, and the enhancement effect of the substrate is enhanced; however, the silver nanostructure is easily oxidized or polluted by molecules to be detected or detection environment in the detection process, the stability is poor, and the storage time is limited. The disclosed methods all use a substrate made of silver nano materials for surface enhancement of Raman spectroscopy, but are deficient in the protection of nano structures, and further research is needed on the number of molecular adsorption and 'hot spots' to be detected.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a silver nano/copper foam material, a preparation method and application thereof, wherein the preparation method adopts a copper foam structure as a frame to improve the stability of a substrate and prolong the storage time limit of the substrate; meanwhile, the prepared silver nano/foamy copper material serving as the SERS substrate improves the adsorption capacity of molecules to be detected, increases the detection hot spots of the substrate, obviously improves the sensitivity of the substrate and reduces the lower detection limit.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of silver nano/foam copper material comprises the following steps:
(1) hydrochloric acid soaking of the foam copper sheet: soaking the cleaned and dried foam copper sheet into a dilute hydrochloric acid solution for a period of time;
(2) removing impurities on the surface of the foam copper sheet: washing the foam copper sheet soaked in the step (1) by using absolute ethyl alcohol and deionized water in sequence to remove impurities on the surface of the foam copper sheet;
(3) preparing a mixed solution: fully mixing the silver nitrate solution and the PVP solution to obtain a mixed solution;
(4) oscillating reaction: immersing the foam copper sheet with the surface removed in the step (2) in the mixed solution obtained in the step (3), and carrying out oscillation reaction for a period of time;
(5) and (3) post-reaction treatment: and (4) washing the foam copper sheet after the oscillation reaction in the step (4) with absolute ethyl alcohol and deionized water in sequence, and then drying to obtain the silver nano/foam copper material.
Preferably, the mass fraction of the dilute hydrochloric acid solution in the step (1) is 3.6%, the dosage is 15mL, and the soaking time is 10 min.
Preferably, the concentration of the silver nitrate solution in the step (3) is 0.1-1 mol/L, and the concentration of the PVP solution is 0.05 g/mL.
Preferably, the volume usage ratio of the silver nitrate solution to the PVP solution in the step (3) is 1: 0.01-0.5.
Preferably, the reaction time in step (4) is 10s to 50s with shaking.
Preferably, the drying temperature in the step (5) is 60 ℃ and the drying time is 2 h.
Still further preferably, the concentration of the silver nitrate solution in the step (3) is 0.8 mol/L.
Still more preferably, the reaction time in step (4) is 40s with shaking.
Meanwhile, the invention also claims the silver nano/foam copper material prepared by the method.
Meanwhile, the invention also claims the application of the silver nano/copper foam material as the SERS substrate.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention creatively provides a silver nano/foam copper material prepared by taking foam copper as a main body frame, and the silver nano/foam copper material can absorb more molecules to be detected and more Raman 'hot spots' by virtue of the three-dimensional structure of the foam copper material, so that Raman enhancement can be greatly promoted, and the sensitivity of SERS detection is improved.
(2) The silver nano/foam copper material prepared by the invention takes the porous rigid structure of the foam copper as the shell, protects the internal silver nano structure, greatly improves the durability and stability of the SERS substrate, and prolongs the storage time limit of the substrate.
(3) The silver nano/foam copper material prepared by the invention uses a foam copper material with lower cost, and the whole preparation process is simple, easy, rapid and easy to master, does not need high-end preparation equipment, and greatly reduces the preparation cost.
(4) The invention unexpectedly discovers that the concentration of the silver nitrate solution and the oscillation time have obvious influence on the performance of the prepared silver nano/foamed copper material, and obtains better process parameters.
Drawings
FIG. 1 shows 0.1M/LAgNO in example 1 of the present invention3SEM images of silver nano/copper foam substrates were formed.
FIG. 2 shows 0.2M/LAgNO in example 2 of the present invention3SEM images of silver nano/copper foam substrates were formed.
FIG. 3 is 0.4M/LAgNO in example 3 of the present invention3SEM images of silver nano/copper foam substrates were formed.
FIG. 4 shows 0.8M/LAgNO in example 4 of the present invention3SEM images of silver nano/copper foam substrates were formed.
FIG. 5 shows 1.6M/LAgNO in example 5 of the present invention3SEM images of silver nano/copper foam substrates were formed.
FIG. 6 shows the use of AgNO at different concentrations in an embodiment of the present invention3The solution is prepared into a Raman spectrogram of the low-concentration 4-ATP probe molecule measured on a silver nanometer/foam copper substrate.
FIG. 7 shows AgNO concentrations in examples of the present invention3And preparing a linear graph of the strongest characteristic peak of the low-concentration 4-ATP probe molecule measured on a silver nano/foam copper substrate by using the solution.
FIG. 8 is an SEM image of the formation of silver nano/foamy copper substrate with 10s shaking time in example 6 of the present invention.
FIG. 9 is an SEM image of the formation of silver nano/foamy copper substrate with 20s oscillation time in example 7 of the present invention.
FIG. 10 is an SEM image of a silver nano/copper foam substrate formed by shaking for 30s in example 8 of the present invention.
FIG. 11 is an SEM photograph of a silver nano/copper foam substrate formed by shaking for 40s in example 9 of the present invention.
FIG. 12 is an SEM image of a silver nano/copper foam substrate formed by shaking for 50s in example 10 of the present invention.
FIG. 13 is a Raman spectrum of a low-concentration 4-ATP probe molecule obtained by using silver nano/copper foam substrates prepared at different oscillation times in examples 6 to 10 of the present invention.
FIG. 14 is a linear graph of the strongest characteristic peak of the low-concentration 4-ATP probe molecule measured on the silver nano/copper foam substrate prepared by different oscillation times in examples 6-10 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly illustrated, the present invention will be further explained in detail with reference to the embodiments and the accompanying drawings.
Unless otherwise specified, the chemical agents used in the present invention are commercially available. Wherein, the thickness of the foam copper sheet adopted by each embodiment of the invention is 0.5mm, and the purity is 99.9%; dilute hydrochloric acid, ethanol, silver nitrate (AgNO)3Purity 99.9%), PVP (polyvinylpyrrolidone) and 4-aminothiophenol (4-ATP, purity not less than 90%) are analytical grade reagents, further purification is not needed, and the used water is deionized water.
Example 1
A preparation method of silver nano/foam copper material comprises the following steps:
(1) hydrochloric acid soaking of the foam copper sheet: soaking the cleaned and dried foam copper sheet with the specification of 0.5cm by 0.5mm into 15mL of dilute hydrochloric acid solution with the mass fraction of 3.6% for 10 min;
(2) removing impurities on the surface of the foam copper sheet: washing the foam copper sheet soaked in the step (1) by using absolute ethyl alcohol and deionized water in sequence to remove impurities on the surface of the foam copper sheet;
(3) preparing a mixed solution: fully mixing 10mL of silver nitrate solution with the concentration of 0.1mol/L with 2mL of 0.05g/mL PVP solution to obtain mixed solution;
(4) oscillating reaction: immersing the foam copper sheet with the surface removed in the step (2) in the mixed solution obtained in the step (3), and carrying out oscillation reaction for 30 s;
(5) and (3) post-reaction treatment: and (4) washing the foam copper sheet after the oscillation reaction in the step (4) with absolute ethyl alcohol and deionized water in sequence, and then putting the foam copper sheet into a vacuum drying oven to be dried for 2 hours at the temperature of 60 ℃ to obtain the silver nano/foam copper material.
Examples 2 to 5
The process conditions and preparation processes of examples 2-5 and example 1 were the same except that the concentration of the silver nitrate solution was different. Wherein, the concentrations of the silver nitrate solutions in the embodiments 2-5 are 0.2mol/L, 0.4mol/L, 0.8mol/L and 1.6mol/L respectively.
FIGS. 1 to 5 are SEM images of silver nano/copper foam materials prepared in examples 1 to 5, respectively, and it can be seen from FIGS. 1 to 5 that AgNO is added3The higher the concentration, the higher the deposition effect of silver nanoparticles on the surface of the copper foam, and the lower the deposition effect.
Meanwhile, the invention uses 10-4The SERS enhancement effect of the silver nano/foam copper substrate prepared in the embodiment 1-5 is tested and analyzed by taking 4-ATP in mol/L as a probe molecule, and the test method is as follows:
(1) the dry clean silver nano/copper foam material was cut into small pieces of appropriate specifications as substrates.
(2) Dropping 10-4And (3) a 4-ATP probe molecular solution of mol/L is used for ensuring that the substrate is fully immersed, and standing for 20min at room temperature.
(3) And (3) placing the substrate after standing into a vacuum drying oven, and drying for 6h at 60 ℃.
(4) The dried sample was subjected to raman spectroscopy.
The test results are shown in fig. 6 and 7. As can be seen from the combination of FIGS. 6 and 7, when AgNO is used3When the concentration is 0.8mol/L, the SERS enhancement effect of the silver nano/foam copper substrate is the best.
Example 6
A preparation method of silver nano/foam copper material comprises the following steps:
(1) hydrochloric acid soaking of the foam copper sheet: soaking the cleaned and dried foam copper sheet with the specification of 0.5cm by 0.5mm into 15mL of dilute hydrochloric acid solution with the mass fraction of 3.6% for 10 min;
(2) removing impurities on the surface of the foam copper sheet: washing the foam copper sheet soaked in the step (1) by using absolute ethyl alcohol and deionized water in sequence to remove impurities on the surface of the foam copper sheet;
(3) preparing a mixed solution: fully mixing 10mL of silver nitrate solution with the concentration of 0.8mol/L with 2mL of 0.05g/mL of PVP solution to obtain mixed solution;
(4) oscillating reaction: immersing the foam copper sheet with the surface removed in the step (2) in the mixed solution obtained in the step (3), and carrying out oscillation reaction for 10 s;
(5) and (3) post-reaction treatment: and (4) washing the foam copper sheet after the oscillation reaction in the step (4) with absolute ethyl alcohol and deionized water in sequence, and then putting the foam copper sheet into a vacuum drying oven to be dried for 2 hours at the temperature of 60 ℃ to obtain the silver nano/foam copper material.
Examples 7 to 10
The process conditions and preparation processes of examples 7 to 10 and 6 were the same except for the shaking time. In examples 7 to 10, the oscillation time was 20s, 30s, 40s, and 50s, respectively.
Fig. 8 to 12 are SEM images of the silver nano/copper foam materials prepared in examples 6 to 10, and it can be seen from the images that the deposition effect of the silver nano particles on the surface of the copper foam is also shown to increase first and then decrease as the oscillation time is gradually increased.
Meanwhile, the invention uses 10-4And (3) testing and analyzing the SERS enhancement effect of the silver nano/foam copper substrate prepared in the embodiment 6-10 by using mol/L4-ATP as a probe molecule, wherein the testing method comprises the following steps:
(1) the dry clean silver nano/copper foam material was cut into small pieces of appropriate specifications as substrates.
(2) Dropping 10-4And (3) ensuring that the substrate is fully immersed by the 4-ATP probe molecular solution of mol/L, and standing for 20min at room temperature.
(3) And (3) placing the substrate after standing into a vacuum drying oven, and drying for 6h at 60 ℃.
(4) The dried sample was subjected to raman spectroscopy.
The test results are shown in fig. 13 and 14. As can be seen from fig. 13 and 14, when the oscillation time is 40s, the SERS enhancement effect of the silver nano/copper foam substrate is the best.
The above description describes the preferred embodiments of the present invention and should not be taken as limiting the scope of the invention as claimed. Any modification, equivalent replacement and improvement without departing from the principle and idea of the present invention should be considered to be within the protection scope of the claims of the present invention.

Claims (6)

1. The application of the silver nano/copper foam material as the SERS substrate is characterized in that the preparation of the silver nano/copper foam material comprises the following steps:
(1) hydrochloric acid soaking of the foam copper sheet: soaking the cleaned and dried foam copper sheet into a dilute hydrochloric acid solution for a period of time;
(2) removing impurities on the surface of the foam copper sheet: washing the foam copper sheet soaked in the step (1) by using absolute ethyl alcohol and deionized water in sequence to remove impurities on the surface of the foam copper sheet;
(3) preparing a mixed solution: fully mixing a silver nitrate solution and a PVP solution to obtain a mixed solution;
(4) oscillating reaction: immersing the foam copper sheet with the surface removed in the step (2) in the mixed solution obtained in the step (3), and carrying out oscillation reaction for a period of time;
(5) and (3) post-reaction treatment: washing the foam copper sheet after the oscillation reaction in the step (4) with absolute ethyl alcohol and deionized water in sequence, and then drying to obtain a silver nano/foam copper material;
wherein the concentration of the silver nitrate solution in the step (3) is 0.8 mol/L;
wherein, the oscillation reaction time in the step (4) is 40 s.
2. The application of the silver nano/copper foam material as the SERS substrate as claimed in claim 1, wherein the mass fraction of the dilute hydrochloric acid solution in the step (1) is 3.6%, the dosage is 15mL, and the soaking time is 10 min.
3. The use of silver nano/copper foam material as a SERS substrate according to claim 1, wherein the concentration of PVP solution in step (3) is 0.05 g/mL.
4. The application of the silver nano/copper foam material as the SERS substrate according to claim 3, wherein the volume usage ratio of the silver nitrate solution to the PVP solution in the step (3) is 1: 0.01-0.5.
5. The application of the silver nano/copper foam material as the SERS substrate according to claim 4, wherein the oscillation reaction time in the step (4) is 10-50 s.
6. The application of the silver nano/foam copper material as the SERS substrate according to any one of claims 1 to 5, wherein the drying temperature in the step (5) is 60 ℃ and the drying time is 2 hours.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101216430A (en) * 2008-01-11 2008-07-09 清华大学 Surface enhanced raman scattering activity nanometer porous metal substrate and method for making same
CN109763119A (en) * 2019-03-01 2019-05-17 西南交通大学 The preparation method of infrared transmission substrate based on displacement reaction
CN110006873A (en) * 2019-04-08 2019-07-12 重庆市环卫集团有限公司 Environmental pollutant detection method based on three-dimensional micro-nano structure enhancing Raman spectrum

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101216430A (en) * 2008-01-11 2008-07-09 清华大学 Surface enhanced raman scattering activity nanometer porous metal substrate and method for making same
CN109763119A (en) * 2019-03-01 2019-05-17 西南交通大学 The preparation method of infrared transmission substrate based on displacement reaction
CN110006873A (en) * 2019-04-08 2019-07-12 重庆市环卫集团有限公司 Environmental pollutant detection method based on three-dimensional micro-nano structure enhancing Raman spectrum

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