CN111679350B - Plasma metal-semiconductor composite film, preparation method thereof and application thereof in non-edible pigment detection - Google Patents

Plasma metal-semiconductor composite film, preparation method thereof and application thereof in non-edible pigment detection Download PDF

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CN111679350B
CN111679350B CN202010588736.0A CN202010588736A CN111679350B CN 111679350 B CN111679350 B CN 111679350B CN 202010588736 A CN202010588736 A CN 202010588736A CN 111679350 B CN111679350 B CN 111679350B
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赵媛
郑芳杰
施丽霞
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Jiangnan University
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Abstract

The invention provides a plasma metal-semiconductor composite film, a preparation method thereof and application thereof in non-edible pigment detection, belonging to the technical field of spectral analysis. The invention mainly comprises the preparation of a plasma metal film and a semiconductor material, wherein a semiconductor ZnGeO: Sr NRs is used for covering the plasma metal film Au @ Ag NP film to prepare the Au @ Ag NP film @ PLMs composite film, and the plasma metal-semiconductor structure can obviously enhance SERS signals, so that the detection of non-edible pigments in food is realized. The plasma metal-semiconductor composite film prepared by the invention can effectively amplify the SERS signal of the analyte and has higher accuracy and sensitivity.

Description

Plasma metal-semiconductor composite film, preparation method thereof and application thereof in non-edible pigment detection
Technical Field
The invention belongs to the technical field of spectral analysis, and particularly relates to a plasma metal-semiconductor composite film, a preparation method thereof and application thereof in non-edible pigment detection.
Background
Industrial dyes generally refer to various dyes used for coloring in industrial production, such as coloring textiles, fur products, wooden products, and ceramic products. The industrial dye has a plurality of varieties, and some illegal vendors resist the temptation of losing profits, and illegally use some industrial dyes to replace edible pigments to be added into food, thereby forming serious threats to human health. Industrial dyes that are widely known for illegal addition to food products include sudan red, rhodamine B, basic yellow pastel, and the like. It is harmful to human body, and many even cause "triogenesis" (teratogenicity, carcinogenesis, mutagenicity).
Generally, SERS techniques use plasmonic metallic materials, especially Au and Ag materials. Recently, SERS studies in 2D NP films have attracted considerable attention. The uniformity of the 2D NP film ensures reproducible SERS signal performance, providing an ideal choice for SERS applications.
More and more semiconductor materials have recently been synthesized, and some of them have been found to produce weak SERS activity. Therefore, a composite material between a semiconductor material and noble metals (Au and Ag) has attracted attention. They may produce a higher SERS effect due to the contribution of electromagnetic enhancement caused by resonance excitation of surface plasmons in NPs and semiconductor-supported chemical enhancement associated with the formation of charge transfer states between noble metals and adjacent semiconductors. Meanwhile, since the semiconductor serving as a dielectric medium blocks attenuation of electromagnetic waves, attenuation of local surface plasmons is suppressed.
Persistent Luminescent Materials (PLMs) capable of storing excitation energy and emitting persistent phosphorescence have also been widely used in various fields, and are emerging promising semiconductor luminescent materials.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a plasma metal-semiconductor composite film, a preparation method thereof and application thereof in non-edible pigment detection. The composite membrane prepared by the invention has good stability and reproducibility, high sensitivity and wide application prospect in the aspect of detecting non-edible pigment in practical application.
The technical scheme of the invention is as follows:
the plasma metal-semiconductor composite film is an Au @ Ag NP film, the semiconductor material is ZnGeO: Sr NRs, and the plasma metal-semiconductor composite film is an Au @ Ag NP film @ PLMs composite film.
A method for preparing a plasma metal-semiconductor composite film, the method comprising the steps of:
(1) preparation of Au @ Ag NP film:
combining AgNO3Adding the solution into Au NPs solution, mixing uniformly, then adding citrate solution and AA (ascorbic acid) solution, mixing uniformly, carrying out solid-liquid separation to obtain Au @ Ag NPs, and dispersing the Au @ Ag NPs in water again to obtain Au @ Ag NPs aqueous solution;
adding hexane into the Au @ Ag NPs aqueous solution obtained in the step I to obtain an immiscible water-hexane interface, adding ethanol into the water-hexane interface, and forming an Au @ Ag NP film at the interface;
(2) preparation of ZnGeO Sr NRs:
(ii) reacting Zn (NO)3)2、Sr(NO3)3Adding the solid to concentrated HNO3Uniformly mixing and stirring the solution, adding water, and uniformly mixing to obtain a colorless and transparent solution 1;
② weighing GeO2Stirring with NaOH and dissolving in water to obtain Na2GeO3A solution;
thirdly, Na obtained in the step II2GeO3Adding the solution into the solution 1 obtained in the step I, uniformly mixing, adjusting the pH value of the solution to 9-10, then carrying out hydrothermal reaction, finally separating to obtain ZnGeO: Sr NRs, and re-dispersing the ZnGeO: Sr NRs in water to finally obtain a ZnGeO: Sr NRs solution;
(3) preparation of Au @ Ag NP film @ PLMs composite film:
and (3) coating the ZnGeO/Sr NRs solution obtained in the step (2) on the Au @ Ag NP film obtained in the step (1) to finally prepare the Au @ Ag NP film @ PLMs composite film.
AgNO described in step (1) ()3The concentration of the solution is 9.8-10.2mM, wherein AgNO3The volume ratio of the solution to the Au NPs solution is 1-3: 40-60; the concentration of the citrate solution is 38-39mM, the concentration of the AA solution is 0.1-0.2M, and the volume ratio of the sodium citrate solution to the AA solution is 15-25: 4-6.
The volume ratio of the Au @ Ag NPs aqueous solution to the hexane in the step (1) is 10-30: 3-5; in the third step (1), the hydrothermal reaction conditions are as follows: heating at 220-225 deg.C for 4-4.5h at a temperature rise rate of 2-2.5 deg.C/min.
The concentration of the concentrated nitric acid in the step (2) is 15.8-16.2mol/L, wherein Zn (NO)3)2、Sr(NO3)3The dosage ratio of the concentrated nitric acid to the water is as follows: 2-2.2mmol, 0.005-0.006mmol, 300-400 μ L, 11-12 mL; na is added in the step (2)2GeO3The volume ratio of the solution to the solution 1 is: 5-15:103-114.
A plasma metal-semiconductor composite film is used for detecting non-edible pigment in food.
The non-edible pigment comprises any one of Sudan red, rhodamine B, basic bright yellow, malachite green, red bright red, lemon yellow, basic orange, quinoline yellow, sunset yellow, amaranth, allura red, new red, acid red, carmine and brilliant blue.
The specific method for detecting the non-edible pigment in the food by using the plasma metal-semiconductor composite film comprises the following steps: adding the solution to be detected into the Au @ Ag NP film @ PLMs composite film, incubating for 12-24h at room temperature, and determining that the wavelength range is 532-785nm Ar-+Raman spectroscopy of ion laser sources.
Preferably, the specific method for detecting the non-edible pigment in the food by using the plasma metal-semiconductor composite film comprises the following steps: dripping the solution to be detected on the Au @ Ag NP membrane, coating the ZnGeO: Sr NRs solution on the Au @ Ag NP membrane, incubating for 12-24h at room temperature, and determining that Ar is 785nm in the wavelength range of 532-+Raman spectroscopy of ion laser sources.
More preferably, the specific method for detecting the non-edible pigment in the food by using the plasma metal-semiconductor composite film comprises the following steps: preparing isometric non-edible pigment standard solutions with different concentration gradients, wherein the concentration range of the standard solution is 10pM-1mM, taking 5-12 concentration gradient values, respectively dripping the standard solutions onto an Au @ Ag NP membrane, incubating at room temperature for 12-24h, coating a ZnGeO: Sr NRs solution on the Au @ Ag NP membrane, and measuring the concentration of Ar at 532-+And obtaining a standard curve by taking the concentration logarithm of the inedible pigment as an abscissa and taking the Raman signal intensity of the inedible pigment as an ordinate through the Raman spectrum of the ion laser source.
The beneficial technical effects of the invention are as follows:
the non-edible pigment detection method provided by the invention has high sensitivity, and the composite membrane has good reproducibility and stability, and can well amplify Raman signals of detected substances.
The Au @ Ag NP film @ PLMs composite film is prepared by covering the Au @ Ag NP film with ZnGeO: Sr film. Au @ Ag NP films with large scale and uniformity were prepared using a hexane-water interface self-assembly process. The stabilized Au @ Ag NP films exhibited amplified SERS signals that originated from hot spots between adjacent NPs. When the Au @ Ag NP film is further covered with a ZnGeO Sr film, the raman signal of the analyte shows more effective enhancement due to charge-transfer between semiconductor-molecules and surface plasmon of the composite material. The Au @ Ag NP film @ PLMs composite film can sensitively detect the inedible pigment in the food by combining the excellent SERS performance, and the detection limit is low. Most importantly, the prepared Au @ Ag NP film @ PLMs composite film has good sensitivity and repeatability, and the huge potential of monitoring the Au @ Ag NP film @ PLMs in complex samples is proved.
Drawings
FIG. 1 is a schematic diagram of the detection of non-edible pigments in the present application.
FIG. 2 is a scanning electron micrograph of the Au @ Ag NP film prepared in example 2.
FIG. 3 is a scanning electron microscope image of the Au @ Ag NP film @ PLMs composite film prepared in example 2.
FIG. 4 shows the Raman spectra and linear relationship of the composite membrane in the presence of different concentrations of Sudan red from example 3.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
A preparation method of a plasma metal-semiconductor composite film for detecting non-edible pigment comprises the following steps:
(1) preparation of Au @ Ag NP film: 100 μ L of 10mM AgNO3The solution was added to 4mL of 15nm Au NPs solution. Next, 150. mu.L of 38.8mM sodium citrate and 40. mu.L of 0.1M AA were poured into the mixture with stirring, and stirred for 15 minutes. After centrifugation, the Au @ Ag NPs were redispersed in 2mL of ultrapure water. 300 μ L of hexane was added to the surface of 1.5mL of the Au @ Ag NPs aqueous solution to form an immiscible water-hexane interface, and ethanol was added dropwise to the surface of the water-hexane layer. Finally the film was carefully transferred to a silicon wafer.
(2) Preparation of ZnGeO Sr NRs: 2.1mmol Zn (NO)3)2，0.0055mmol Sr(NO3)3With 350 μ L concentrated HNO3Mixed under vigorous stirring, and 11.5mL of ultrapure water was added thereto to form a colorless transparent solution. 1.45g of GeO are weighed2And 1.65g NaOH dissolved in 21mL of ultrapure water, and continuously stirring for 7h until the solution is clear to obtain Na2GeO3And (3) solution. 1.75mL of Na obtained by the preparation2GeO3Adding the solution into the solution dropwise, adjusting pH to 9.5 by adding ammonia water, gradually changing the solution from clear to white turbid, continuously and rapidly stirring at room temperature for 1h, transferring into a polytetrafluoroethylene hydrothermal reaction kettle, heating to 220 deg.C for 4h, and heating at a rate of 220 deg.CAt 2 deg.C/min. Finally, the ZnGeO: Sr NRs were centrifuged and dispersed in water for further use.
(3) Preparation of Au @ Ag NP film @ PLMs composite film:
prepared Sudan red standard solutions with the concentrations of 10pM, 100pM, 1nM, 10nM, 100nM, 1. mu.M, 10. mu.M, 100. mu.M and 1mM are respectively dripped onto the Au @ Ag NP membrane and incubated at room temperature for 12 h. A20 μ L solution of ZnGeO Sr NRs was then coated onto the Au @ Ag NP film. By using 785nm Ar at room temperature+And a Raman spectrometer of the ion laser source measures Raman spectrum. Through the series of concentration Raman spectrum measurement, a standard curve taking the logarithm of the concentration of the inedible pigment as the abscissa and the Raman signal intensity of the inedible pigment as the ordinate is obtained.
Example 2
A preparation method of a plasma metal-semiconductor composite film for detecting non-edible pigment comprises the following steps:
(1) preparation of Au @ Ag NP film: 200 μ L of 10mM AgNO3The solution was added to 5mL of 15nm Au NPs solution. Next, 200. mu.L of 38.8mM sodium citrate and 50. mu.L of 0.1M AA were poured into the mixture with stirring, and stirred for 15 minutes. After centrifugation, the Au @ Ag NPs were redispersed in 2mL of ultrapure water. 400 μ L of hexane was added to the surface of 2mL of the Au @ Ag NPs aqueous solution to form an immiscible water-hexane interface, and ethanol was added dropwise to the surface of the water-hexane layer. Finally the film was carefully transferred to a silicon wafer.
(2) Preparation of ZnGeO Sr NRs: 2mmol Zn (NO)3)2，0.005mmol Sr(NO3)3With 300. mu.L concentrated HNO3Mixed under vigorous stirring, and 11mL of ultrapure water was added thereto to form a colorless transparent solution. Weighing 1.3g GeO2And 1.5g NaOH dissolved in 21mL of ultrapure water, and continuously stirring for 7h until the solution is clear to obtain Na2GeO3And (3) solution. 1.5mL of Na obtained by the preparation2GeO3Adding the solution into the solution dropwise, adjusting the pH value of the solution to 9.5 by adding ammonia water, gradually changing the solution from clear to white and turbid, continuously and rapidly stirring at room temperature for 1h, and transferring the solution into a polytetrafluoroethylene hydrothermal reaction kettleHeating the mixture for 4 hours when the temperature is raised to 220 ℃, wherein the temperature raising rate is 2 ℃/min. Finally, the ZnGeO: Sr NRs were centrifuged and dispersed in water for further use.
(3) Preparation of Au @ Ag NP film @ PLMs composite film:
prepared Sudan red standard solutions with the concentrations of 10pM, 100pM, 1nM, 10nM, 100nM, 1. mu.M, 10. mu.M, 100. mu.M and 1mM are respectively dripped onto the Au @ Ag NP membrane and incubated at room temperature for 12 h. A20 μ L solution of ZnGeO Sr NRs was then coated onto the Au @ Ag NP film. By using 785nm Ar at room temperature+And a Raman spectrometer of the ion laser source measures Raman spectrum. Through the series of concentration Raman spectrum measurement, a standard curve taking the logarithm of the concentration of the inedible pigment as the abscissa and the Raman signal intensity of the inedible pigment as the ordinate is obtained.
Example 3
A preparation method of a plasma metal-semiconductor composite film for detecting non-edible pigment comprises the following steps:
(1) preparation of Au @ Ag NP film: 300 μ L of 10mM AgNO3The solution was added to 6mL of 15nm Au NPs solution. Next, 250. mu.L of 38.8mM sodium citrate and 60. mu.L of 0.1M AA were poured into the mixture with stirring, and stirred for 15 minutes. After centrifugation, the Au @ Ag NPs were redispersed in 2mL of ultrapure water. 500 μ L of hexane was added to the surface of 2.5mL of the Au @ Ag NPs aqueous solution to form an immiscible water-hexane interface, and ethanol was added dropwise to the surface of the water-hexane layer. Finally the film was carefully transferred to a silicon wafer.
(2) Preparation of ZnGeO Sr NRs: 2.2mmol Zn (NO)3)2，0.006mmol Sr(NO3)3With 400 μ L concentrated HNO3Mixed under vigorous stirring, and 12mL of ultrapure water was added thereto to form a colorless transparent solution. 1.6g of GeO are weighed2And 1.8g NaOH dissolved in 21mL of ultrapure water, and continuously stirring for 7h until the solution is clear to obtain Na2GeO3And (3) solution. 2mL of Na obtained by the preparation2GeO3Adding the solution dropwise into the above solution, adjusting pH to 9.5 by adding ammonia water, gradually changing the solution from clear to white turbid, and continuously and rapidly adding ammonia water at room temperatureStirring for 1h, transferring into a polytetrafluoroethylene hydrothermal reaction kettle, heating to 220 ℃ and heating for 4h, wherein the heating rate is 2 ℃/min. Finally, the ZnGeO: Sr NRs were centrifuged and dispersed in water for further use.
(3) Preparation of Au @ Ag NP film @ PLMs composite film:
prepared Sudan red standard solutions with the concentrations of 10pM, 100pM, 1nM, 10nM, 100nM, 1. mu.M, 10. mu.M, 100. mu.M and 1mM are respectively dripped onto the Au @ Ag NP membrane and incubated at room temperature for 12 h. A20 μ L solution of ZnGeO Sr NRs was then coated onto the Au @ Ag NP film. By using 785nm Ar at room temperature+And a Raman spectrometer of the ion laser source measures Raman spectrum. Through the series of concentration Raman spectrum measurement, a standard curve taking the logarithm of the concentration of the inedible pigment as the abscissa and the Raman signal intensity of the inedible pigment as the ordinate is obtained.

Claims (10)

1. The plasma metal-semiconductor composite film is characterized in that the plasma metal film is an Au @ Ag NP film, the semiconductor material is ZnGeO: Sr NRs, and the plasma metal-semiconductor composite film is an Au @ Ag NP film @ PLMs composite film.
2. A method for preparing a plasma metal-semiconductor composite film according to claim 1, comprising the steps of:
(1) preparation of Au @ Ag NP film:
combining AgNO3Adding the solution into Au NPs solution, mixing uniformly, then adding citrate solution and ascorbic acid AA solution, mixing uniformly, carrying out solid-liquid separation to obtain Au @ Ag NPs, and dispersing the Au @ Ag NPs in water again to obtain Au @ Ag NPs aqueous solution;
adding hexane into the Au @ Ag NPs aqueous solution obtained in the step I to obtain an immiscible water-hexane interface, adding ethanol into the water-hexane interface, and forming an Au @ Ag NP film at the interface;
(2) preparation of ZnGeO Sr NRs:
(ii) reacting Zn (NO)3)2、Sr(NO3)3Adding the solid to concentrated HNO3Mixing and stirring the solution evenlyMixing, adding water, and mixing to obtain colorless transparent solution 1;
② weighing GeO2Stirring with NaOH and dissolving in water to obtain Na2GeO3A solution;
thirdly, Na obtained in the step II2GeO3Adding the solution into the solution 1 obtained in the step I, uniformly mixing, adjusting the pH value of the solution to 9-10, then carrying out hydrothermal reaction, finally separating to obtain ZnGeO: Sr NRs, and re-dispersing the ZnGeO: Sr NRs in water to finally obtain a ZnGeO: Sr NRs solution;
(3) preparation of Au @ Ag NP film @ PLMs composite film:
and (3) coating the ZnGeO/Sr NRs solution obtained in the step (2) on the Au @ Ag NP film obtained in the step (1) to finally prepare the Au @ Ag NP film @ PLMs composite film.
3. The method for preparing a plasma metal-semiconductor composite film according to claim 2, wherein AgNO is used in the step (1): wherein AgNO is used as a precursor3The concentration of the solution is 9.8-10.2 moL/m3Wherein AgNO3The volume ratio of the solution to the Au NPs solution is 1-3: 40-60; the concentration of the citrate solution is 38-39 moL/m3AA concentration of 1X 102-2×102moL/m3Wherein the volume ratio of the sodium citrate solution to the ascorbic acid AA solution is 15-25: 4-6.
4. The method for preparing a plasma metal-semiconductor composite film according to claim 2, wherein the ratio of the amount of the Au @ Ag NPs aqueous solution to the amount of hexane used in the step (1) is 10-30:3-5 by volume; in the third step (1), the hydrothermal reaction conditions are as follows: heating at 220-225 deg.C for 4-4.5h at a temperature rise rate of 2-2.5 deg.C/min.
5. The method for preparing a plasma metal-semiconductor composite film according to claim 2, wherein the concentration of the concentrated nitric acid in the (2) step (1) is 15.8 to 16.2mol/L, in which Zn (NO) is present3)2、Sr(NO3)3Concentrated nitric acid andthe dosage ratio of water is as follows: 2-2.2mmol, 0.005-0.006mmol, 300-400 μ L, 11-12 mL; na is added in the step (2)2GeO3The volume ratio of the solution to the solution 1 is: 5-15:103-114.
6. A method for detecting a non-edible pigment in a food, which comprises applying the plasma metal-semiconductor composite film as defined in claim 1.
7. The use according to claim 6, wherein the non-food coloring comprises any one of Sudan red, rhodamine B, basic Bright yellow, Malachite Green, Red Bright Red, lemon yellow, basic orange, quinoline yellow, sunset yellow, amaranth, allura Red, New Red, acid Red, carmine and Brilliant blue.
8. The application of claim 6, wherein the specific method for detecting the non-edible pigment in the food by using the plasma metal-semiconductor composite film comprises the following steps: adding the solution to be detected into the Au @ Ag NP film @ PLMs composite film, incubating for 12-24h at room temperature, and determining that the wavelength range is 532-785nm Ar-+Raman spectroscopy of ion laser sources.
9. The application of claim 8, wherein the specific method for detecting the non-edible pigment in the food by using the plasma metal-semiconductor composite film is as follows: dripping the solution to be detected on the Au @ Ag NP membrane, coating the ZnGeO: Sr NRs solution on the Au @ Ag NP membrane, incubating for 12-24h at room temperature, and determining that Ar is 785nm in the wavelength range of 532-+Raman spectroscopy of ion laser sources.
10. The application of the plasma metal-semiconductor composite film according to claim 9, wherein the specific method for detecting the non-edible pigment in the food by using the plasma metal-semiconductor composite film is as follows: preparing isometric non-edible pigment standard solution with different concentration gradients, wherein the concentration range of the standard solution is 10-8 moL/m3-1 moL/m3Taking 5-12 concentration gradient values, and then respectively dropwise adding the standard solution to Au @ AgIncubating for 12-24h at room temperature on NP membrane, coating ZnGeO Sr NRs solution on Au @ Ag NP membrane, and determining Ar at 532-785nm+And obtaining a standard curve by taking the concentration logarithm of the inedible pigment as an abscissa and taking the Raman signal intensity of the inedible pigment as an ordinate through the Raman spectrum of the ion laser source.
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