CN110967332A - Raman enhanced active substrate with directional extraction and oil phase solution concentration, and preparation method and application thereof - Google Patents
Raman enhanced active substrate with directional extraction and oil phase solution concentration, and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of Raman detection, and particularly relates to a Raman enhanced active substrate with directional extraction and oil phase solution concentration, and a preparation method and application thereof. The method comprises the following steps: (1) soaking the copper mesh by using a solution containing hypochlorite radicals to grow copper oxide nanowires on the surface of the copper mesh; (2) and thermally evaporating a Raman signal enhancement layer on the surface of the copper mesh on which the copper oxide nanowires grow, and then carrying out infrared lamp irradiation treatment to obtain the copper mesh. According to the invention, through the capillary action of the metal oxide nanowires growing in situ on the surface of the copper mesh and the hydrophobic action of the irradiated rough surface, the oil phase can move upwards along the nanowires and is continuously evaporated, so that separation, directional extraction and concentration of the oil phase are generated, a detection signal is enhanced, the sensitivity is improved, and the substrate provided by the invention can be used for directly detecting oil phase pollutants in a mixed phase without separating or directionally extracting liquid to be detected in advance through separation treatment.
Description
Technical Field
The invention belongs to the technical field of Raman detection, and particularly relates to a Raman enhanced active substrate with directional extraction and oil phase solution concentration, and a preparation method and application thereof.
Background
The information disclosed in this background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Today, toxic organic compounds (e.g., dyes and herbicides) used in agriculture and industry are a source of environmental pollution. Effective detection means are required to avoid damage to the society. However, many contaminants are only soluble in the oil phase and not in the water phase, and they are often difficult to detect in routine testing because the oil and water phases are not soluble. Although many methods are available for detection, such as high performance liquid chromatography, these methods are often too complex and costly and difficult to accurately detect. In addition, for water pollution detection, highly sensitive detection of pollutants is an important point. The Surface Enhanced Raman Spectroscopy (SERS) is widely used due to high sensitivity, simple sample preparation process, rapid detection mode, accuracy and non-invasiveness, and has wide application prospect in environmental pollution detection.
However, for conventional raman detection, the most commonly used dropping method and soaking method of the detection liquid cannot ensure that the liquid to be detected is uniformly distributed on the raman substrate, so that the reliability of the raman signal is greatly reduced. Although extraction methods and the like can be used for separating or directionally extracting the liquid to be measured in advance, the method also means that a great deal of extra time and cost are needed, and the liquid to be measured can be influenced in the separation process. This is an important reason that hinders the popularity of SERS in contaminant detection.
Disclosure of Invention
Aiming at the problems, the invention provides the Raman enhanced active substrate with the functions of directional extraction and oil phase solution concentration, and the preparation method and the application thereof.
The first object of the present invention: a raman-enhanced active substrate with a directionally extracted, concentrated oil phase solution is provided.
Second object of the invention: provides a preparation method of a Raman enhanced active substrate with directional extraction and oil phase solution concentration.
The third object of the present invention: applications of the raman-enhanced active substrate with a directionally extracted, concentrated oil phase solution are provided.
In order to realize the purpose, the invention discloses the following technical scheme:
first, the present invention discloses a raman-enhanced active substrate with a directionally extracted, concentrated oil phase solution, comprising: the Raman signal enhancement layer comprises a copper net, copper oxide nanowires and a Raman signal enhancement layer; the nanowires grow on the surface of the copper mesh in situ, the Raman signal enhancement layer is attached to the surfaces of the copper mesh and the copper oxide nanowires, and the substrate has a hydrophobic function.
Further, the copper mesh includes any one of a red copper mesh, a brass mesh, a phosphor copper mesh, and the like, and correspondingly, the nanowires are copper oxide nanowires. It should be noted that the growing of nanowires is not a commonality of metals, which is a special property that is biased to be possessed by a few metals according to the current research of the present invention, and a metal oxide with a nanowire-like morphology cannot be easily grown in situ on any metal.
Further, the mesh of the copper net is 100-300 meshes.
Further, the raman signal enhancing layer includes silver plating, gold plating, platinum plating, or the like. Optionally, the plating layer is obtained by evaporation.
Further, the nanowire refers to a metal oxide having a diameter of a columnar structure reaching a nano scale, and the length thereof may not be in the nano scale range.
Secondly, the invention discloses a preparation method of a Raman enhanced active substrate with directional extraction and oil phase solution concentration, which comprises the following steps:
(1) soaking the copper mesh by using a solution containing hypochlorite radicals to grow copper oxide nanowires on the surface of the copper mesh;
(2) and thermally evaporating a Raman signal enhancement layer on the surface of the copper mesh on which the copper oxide nanowires grow, and then carrying out infrared lamp irradiation treatment to obtain the copper mesh. Raman signals can be increased through the Raman signal enhancement layer, and then the surface of the substrate becomes hydrophobic through infrared lamp irradiation treatment, so that the oil phase solution can be directionally extracted.
Further, in the step (1), the hypochlorite solution has a hypochlorite content of 10-30% by volume, and optionally, the hypochlorite solution includes a hypochlorous acid solution, a sodium hypochlorite solution, and the like.
Further, in the step (1), when the soaking time is 80-150s, the processing time within the range can ensure that the morphology of the copper oxide nanowires is more suitable for concentration of oil phase molecules.
Further, in the step (2), the thermal evaporation conditions are as follows: the evaporation current is 65-72A, the deposition rate is 0.1-0.25nm/s, and the deposition time is 70-110 s.
Further, in the step (2), the conditions of the infrared lamp irradiation treatment are as follows: the power is 260-285W, the irradiation treatment time is 5.5-6.5h, and the distance between the infrared lamp and the copper net is 30-42 cm.
Further, in the step (1), before soaking, the method further comprises a step of pretreating the copper mesh, specifically: sequentially washing the copper net with acetone, ethanol and deionized water, and then immersing the copper net in dilute sulfuric acid to remove surface oxides, so as to avoid influencing the appearance of the copper oxide nanowires; then rinsed with deionized water and ethanol and dried.
Thirdly, the invention discloses a method for detecting the oil phase in the mixed solution by adopting the substrate, which comprises the following steps: and folding the Raman substrate into a boat shape, placing and floating on the surface of the oil-water mixed solution to be detected, standing for a period of time to enable the oil phase to be immersed into the boat, and then detecting the Raman spectrum of the substrate.
Secondly, the invention discloses a detection method for the substrate after the oil phase in the mixed solution is concentrated, which comprises the following steps: the Raman substrate is folded into a boat shape, placed on a floating water surface, a plurality of drops of oil phase to be detected are dropped on the water surface, the boat can spontaneously suck oil into the boat through the vicinity, the oil sucked into the boat is evaporated (the oil is quickly evaporated when the oil is less than that of the oil dropped each time, the oil is dropped once after the oil is completely evaporated, and probe molecules in the oil are continuously accumulated on the substrate in the circulating process), the plurality of drops of oil phase solution are dropped again after the oil is completely evaporated, and the Raman spectrum of the substrate is detected after the oil phase solution is circulated for a plurality of times.
Finally, the invention discloses the Raman enhancement active substrate with the directional extraction and oil phase solution concentration function and the application of the substrate obtained by the preparation method of the Raman enhancement active substrate with the directional extraction and oil phase solution concentration function in the field of environmental detection.
Compared with the prior art, the invention has the following beneficial effects:
(1) experiments prove that the Raman enhanced active substrate for self-separating multiphase mixed solution prepared by the invention does not need to separate or directionally extract the liquid to be detected after separation treatment in advance, so that the detection can be directly carried out on the multiphase mixed solution, the detection sensitivity is higher, and the minimum detection concentration of the Raman enhanced active substrate for the self-separating multiphase mixed solution can reach 10-10M。
(2) The substrate is made hydrophobic through infrared irradiation, so that the water phase and the oil phase selectively pass through the substrate, the pollutants in the oil phase in the mixed phase are directionally detected, and meanwhile, the concentration of the oil phase is realized due to the characteristic, and a higher detection limit is realized.
(3) According to the invention, through the capillary action of the metal oxide nanowires growing in situ on the surface of the copper mesh and the hydrophobic action of the irradiated rough surface, the oil phase can move upwards along the nanowires and is continuously evaporated, so that separation, directional extraction and concentration of the oil phase are generated, a detection signal is enhanced, the sensitivity is improved, and the substrate provided by the invention can be used for directly detecting oil phase pollutants in a mixed phase without separating or directionally extracting liquid to be detected in advance through separation treatment.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is an SEM image of a raman-enhanced active substrate prepared in example 1 of the present invention.
Fig. 2 is an image of an energy dispersive spectrometer of a raman enhanced active substrate prepared in example 1 of the present invention.
Fig. 3 shows raman spectra of different concentrations of R6G on raman-enhanced active substrates prepared in example 1.
FIG. 4 shows the concentration 10-6R6G for M613 cm in Raman spectrum on Raman enhanced active substrate prepared in example 1-1Characteristic peak intensity of (2).
Fig. 5 is a graph showing the effect of the raman-enhanced active substrate prepared in example 1 of the present invention in directionally absorbing the oil phase solution.
Fig. 6 is a raman spectrum detected after the raman-enhanced active substrate prepared in example 1 of the present invention concentrates the oil phase solution.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The defects of a small amount of oil phase solution included in the multiphase mixed solution are difficult to detect by the conventional SERS. Therefore, the invention provides the Raman enhanced active substrate with the directional extraction and oil phase solution concentration and the preparation method thereof; the invention will now be further described with reference to the drawings and detailed description.
In the following examples, the materials used were: acetone (CH)3COCH3AR, 99.5%), alcohol (C)2H5OH, 99.7%), Sudan I (C)16H12N2O, AR) and amphetamine (NaClO, CP) were purchased from national drug stock chemical agents limited.
Silver particles (99.99%), a purple copper mesh (200 meshes), rhodamine 6G (C)28H31N2O3Cl, AR), malachite green (C)23H25N2·C2HO4·0.5C2H2O4AR) and toluene (C)7H8AR, 99.5%) was purchased from Sigma-Aldrich.
Example 1
Preparation of a Raman enhanced active substrate with directional extraction and oil phase solution concentration, comprising the following steps:
(1) and (3) growth of copper oxide nanowires: the 200 mesh violet copper mesh was washed with acetone, ethanol and deionized water in that order for 10 minutes, after which the copper mesh was immersed in sulfuric acid (0.25M) for 10 minutes to remove surface oxides, then rinsed with deionized water and ethanol and dried. The cleaned copper net is immersed in a diluted antipyrine solution (25% of volume fraction) for 100 seconds, and copper oxide nanowires grow on the copper net. Then rinsed with alcohol and dried.
(2) Thermally evaporating the silver coating: a thin layer of silver was deposited on the surface of the copper mesh by thermal evaporation. The evaporation material was high purity Ag particles, the evaporation current was 70A, the deposition rate was set to 0.1nm/s, and the deposition time was 100 s.
(3) Treating wettability: placing the copper net deposited with the silver layer under an infrared lamp for irradiation, wherein the power is 275W, and the distance between the copper net and the lamp is 35 cm; and obtaining the Raman enhanced active substrate after 6h of irradiation.
Example 2
Preparation of a Raman enhanced active substrate with directional extraction and oil phase solution concentration, comprising the following steps:
(1) and (3) growth of copper oxide nanowires: the 300 mesh violet copper mesh was washed with acetone, ethanol and deionized water in that order for 10 minutes, after which the copper mesh was immersed in sulfuric acid (0.25M) for 8 minutes to remove surface oxides, then rinsed with deionized water and ethanol and dried. And (3) soaking the cleaned copper net in a diluted antipyrine solution (30% of volume fraction) for 80 seconds to grow copper oxide nanowires on the copper net. Then rinsed with alcohol and dried.
(2) Thermal evaporation of gold plating layer: a thin layer of gold is deposited on the surface of the copper mesh by thermal evaporation. The evaporation material was high-purity Au particles, the evaporation current was 65A, the deposition rate was set to 0.2nm/s, and the deposition time was 110 s.
(3) Treating wettability: placing the copper mesh on which the gold layer is deposited under an infrared lamp for irradiation, wherein the power is 285W, and the distance between the copper mesh and the lamp is 30 cm; and obtaining the Raman enhanced active substrate after 5.5h of irradiation.
Example 3
Preparation of a Raman enhanced active substrate with directional extraction and oil phase solution concentration, comprising the following steps:
(1) and (3) growth of copper oxide nanowires: the 100 mesh violet copper mesh was washed with acetone, ethanol and deionized water in that order for 10 minutes, after which the copper mesh was immersed in sulfuric acid (0.25M) for 10 minutes to remove surface oxides, then rinsed with deionized water and ethanol and dried. And soaking the cleaned copper net in a diluted antipyrine solution (10% of volume fraction) for 150 seconds to grow copper oxide nanowires on the copper net. Then rinsed with alcohol and dried.
(2) Thermally evaporating the silver coating: a thin layer of silver was deposited on the surface of the copper mesh by thermal evaporation. The evaporation material was high purity Ag particles, the evaporation current was 72A, the deposition rate was set to 0.25nm/s, and the deposition time was 70 s.
(3) Treating wettability: placing the copper net deposited with the silver layer under an infrared lamp for irradiation, wherein the power is 260W, and the distance between the copper net and the lamp is 42 cm; and obtaining the Raman enhanced active substrate after 6.5h of irradiation.
Effect testing：
Take the raman-enhanced active substrate prepared in example 1 as an example. The substrate was characterized and examined and the results are shown in fig. 1-6. Wherein:
fig. 1 is an SEM image of the raman-enhanced active substrate, and it can be seen that: the surface of the copper mesh is uniformly grown with nano beams.
Fig. 2 is an image of an energy dispersion spectrometer of the raman enhanced active substrate, which can be proved to be CuO and Ag, and several elements are uniformly distributed.
In order to further verify the sensitivity and uniformity of the raman-enhanced active substrate prepared in example 1, a commonly used alcohol solution of R6G was selected as a probe molecule in the present invention. Each time, 4. mu.l of the solution was dropped on the substrate, and the test was performed after it was naturally dried. Raman measurements were performed using Raman confocal microscopy (LabRAM HR Evolution). The parameters are set to obtain signals every 8s, the detector is repeatedly exposed twice, real-time collected images are displayed every second, the light intensity is set to be 0.48mW, the wavelength of laser is 532nm, and the grating is set to be 1800 gr/mm.
FIG. 3 shows the concentration of 10-6M、10-8M、10-10Raman spectroscopy of R6G of M on the Raman-enhanced active substrate, demonstrated at concentrations as low as 10-10The characteristic peak of R6G can still be clearly measured in the case of M.
FIG. 4 shows that the concentration of the Raman-enhanced active substrate surface is 10 when fifteen random positions are taken-6613cm in Raman spectrum of R6G of M-1The characteristic peak intensity of the Raman spectrum sensor proves to have high uniformity, wherein the uniformity refers to the difference of the test performance of the whole substrate at different positions, the diameter of a Raman light spot is about one micron, namely, only a very small point on the substrate can be selected for obtaining a signal in each measurement, and if the performance difference of different areas of the surface of the substrate is large, the test result cannot be accurately fed back in the test process. For example, the same solution is tested with the same substrate, because it cannot be guaranteed that each measurement is at the same location, if the substrate is not uniform, three distinct conclusions may be drawn from the three tests; therefore, the high uniformity can make the test result stable and reliable.
Referring to FIG. 5, to demonstrate the directional uptake of the oil phase solution by the substrate, the present invention drops 4mL of toluene into water, which is stained with Sudan Red (Sudan I) for ease of differentiation. The copper mesh substrate was then folded into a boat shape and placed on its surface. Since it was previously illuminated by an infrared lamp and the substrate was hydrophobic, water could not enter the boat and only toluene could enter the boat. When the boat was placed in a petri dish containing 20mL of deionized water and 4mL of toluene, it was observed that toluene floating on the water surface was immediately sucked into the interior of the boat. Toluene can be simply transferred out by a pipette and after 60 seconds, the boat is removed and the mixture is again observed, and virtually no residual toluene is found. This demonstrates that the use of the substrate to separate and extract the oil phase is effective.
To demonstrate that the substrate also had a thickening effect on the oil phase, the present invention was floated on the water surface using the above-described boat and 1mL of 10 concentration solution was dropped next to the boat-6M sudan I in toluene, wait for it to dry and take out the boat and measure its raman signal. Thereafter, the boat is returned to the surface and the above steps are repeated. Because of the capillary action of the CuO nanowires, toluene will move up the wire and evaporate continuously, and cause the more oil red molecules dissolved therein to gather on the wire. The more cycles, the stronger the raman signal. As shown in fig. 6, raman spectra measured for one drop, five drops, and twenty drops, demonstrate that the substrates prepared according to the present invention do have excellent condensation.
It should be noted that, when liquid is detected by raman, the existing method usually extracts probe molecules by a dropping method or a soaking method; the test is carried out after the solution to be tested has dried. The gaps between the copper oxide nanowires of the present invention allow the liquid to spontaneously flow up the nanowires, climbing from the low end to the high end of the nanowires. Because the oil phase on the line is continuously evaporated to a gaseous state, the oil at the bottom of the line will continue to replenish the line. In the process, molecules dissolved in the oil are brought to the line in a large amount, and probe molecules in the oil are continuously accumulated on the substrate in the circulation process, so that the oil phase is concentrated.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A raman-enhanced active substrate with a directional extraction, concentrated oil phase solution, comprising: the Raman signal enhancement layer comprises a copper net, copper oxide nanowires and a Raman signal enhancement layer; the nanowires grow on the surface of the copper mesh in situ, the Raman signal enhancement layer is attached to the surfaces of the copper mesh and the copper oxide nanowires, and the substrate has a hydrophobic function.
2. A raman-enhanced active substrate with a directional extraction, concentrated oil phase solution according to claim 1 wherein said copper mesh comprises any one of a violet copper mesh, a brass mesh, a phosphor copper mesh.
3. A raman-enhanced active substrate with a directionally-extracted, concentrated oil-phase solution according to claim 1, wherein said raman signal enhancement layer comprises any one of silver plating, gold plating, platinum plating.
4. The Raman-enhanced active substrate with oriented extraction and oil-phase solution concentration function as claimed in any one of claims 1 to 3, wherein the mesh of the copper mesh is 100-300 meshes.
5. A method for preparing a Raman-enhanced active substrate with a directionally-extracted, concentrated oil-phase solution according to any one of claims 1 to 4, comprising the steps of:
(1) soaking the copper mesh by using a solution containing hypochlorite radicals to grow copper oxide nanowires on the surface of the copper mesh;
(2) and thermally evaporating a Raman signal enhancement layer on the surface of the copper mesh on which the copper oxide nanowires grow, and then carrying out infrared lamp irradiation treatment to obtain the copper mesh.
6. A method for preparing a Raman-enhanced active substrate having a directionally-extracted, concentrated oil-phase solution according to claim 5, wherein in step (1), the hypochlorite solution contains hypochlorite in an amount of 10 to 30% by volume; preferably, the hypochlorite-containing solution comprises a hypochlorous acid solution or a sodium hypochlorite solution;
preferably, in the step (1), the soaking time is 80-150 s.
7. A method for preparing a Raman enhanced active substrate with a directional extraction and oil phase concentration solution according to claim 5, wherein preferably, in the step (2), the thermal evaporation conditions are as follows: the evaporation current is 65-72A, the deposition rate is 0.1-0.25nm/s, and the deposition time is 70-110 s;
preferably, in the step (2), the conditions of the infrared lamp irradiation treatment are as follows: the power is 260-285W, the irradiation treatment time is 5.5-6.5h, and the distance between the infrared lamp and the copper net is 30-42 cm;
preferably, in the step (1), before the soaking, the method further comprises a step of pretreating the copper mesh: sequentially washing the copper mesh by using acetone, ethanol and deionized water, and then immersing the copper mesh into dilute sulfuric acid to remove surface oxides; then rinsed with deionized water and ethanol and dried.
8. A method for detecting an oil phase in a mixed solution, which is carried out by using a raman-enhanced active substrate according to any one of claims 1 to 4 and/or a substrate prepared by the method according to any one of claims 5 to 7, comprising the steps of: and folding the Raman substrate into a boat shape, placing and floating on the surface of the oil-water mixed solution to be detected, standing for a period of time to enable the oil phase to be immersed into the boat, and then detecting the Raman spectrum of the substrate.
9. A method for detecting an oil phase in a concentrated mixed solution, which is carried out by using a raman-enhanced active substrate according to any one of claims 1 to 4 and/or a substrate prepared by the method according to any one of claims 5 to 7, comprising the steps of: the Raman substrate is folded into a boat shape, placed on and floated on the water surface, a few drops of oil phase to be detected are dropped on the water surface, the boat can spontaneously suck the oil into the interior through the vicinity, a few drops of oil phase solution are dropped again after the oil phase solution is completely evaporated, and the Raman spectrum of the substrate is detected after circulation for a plurality of times.
10. Use of a raman-enhanced active substrate according to any one of claims 1 to 4 and/or a substrate prepared according to the method of any one of claims 5 to 7 in the field of environmental detection.
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| CN102181891A (en) * | 2011-04-08 | 2011-09-14 | 温州大学 | Silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and preparation method and application thereof |
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