CN114324292B - Method and equipment for calibrating nondestructive quality inspection of silver or gold nanoparticle film Raman chip - Google Patents
Method and equipment for calibrating nondestructive quality inspection of silver or gold nanoparticle film Raman chip Download PDFInfo
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Abstract
A Raman chip calibration nondestructive quality inspection method and equipment for silver or gold nanoparticle films, wherein the Raman chip detects Extinction (extraction) absorption spectrum SPR main peak height H in ultraviolet visible parallel light beams SPR By H SPR ～H Rs Calibration method using the height H of the calibration peak in the Raman spectrum of the calibration sample RS Indirectly characterizing the sensitivity quality of the raman chip; h SPR ～H RS Calibration curve, H with at least 5 different sensitivities to be detected SPR After the values, the calibration samples, e.g. R6g-10, are successively examined ‑6 Scaled peak height H in the Raman spectrum of M/L RS Create H SPR ～H RS And (3) a calibration curve, namely, a quality control limit is manufactured according to the standard of the quality inspection of the Raman chip, and the Raman chip calibration nondestructive quality inspection is implemented. In the nondestructive quality inspection process, in order to prevent the Raman chip from being damaged by oxidation in the air, the Raman chip needs to be arranged in a silver nitrate solution environment, or in a vacuum environment or in inert gas.
Description
Technical Field
The invention relates to the field of SERS Raman spectrum chips in Raman spectrum analysis technology, in particular to a method and equipment for calibrating nondestructive quality inspection of a silver or gold nanoparticle film Raman chip.
Background
Currently, a sample with higher Raman activity is selected by using a SERS Raman chip (RS chip or Raman chip for short) sensitivity quality detection of a silver or gold nanoparticle film, for example, an R6g aqueous solution with the concentration of micro-nano M/L is adopted as a standard sample, the sample is placed on a Raman chip, placed on a sample stage of a deep refrigeration-CCD Raman spectrometer, and the Raman spectrum of R6g molecules is detected and used as a reference standard for checking the sensitivity quality of the Raman chip. Because the sensitivity of the Raman chip is very high, and the Raman chip is difficult to clean after being used for detection once, the Raman chip cannot be used for the second ultra-high-sensitivity detection multiplexing. Therefore, when the Raman chip products are subjected to delivery quality inspection, the 'spot inspection' can be implemented only in the same batch of products, and no nondestructive quality inspection method and equipment for the silver or gold nanoparticle film Raman chips exist. In the industrial development of the raman chip, in order to ensure that each product is subjected to 'factory quality inspection', a nondestructive quality inspection method and equipment of a silver or gold nanoparticle film raman chip need to be developed.
The inventor Wu Shifa in 2004 directs the research institute Li Yaqin to release "international conference paper for photoelectron and spectrum of Beijing nanostructures and materials, SPIE,5635:31-37", the structural raman chip of the trimeric type-silver foil/silver nanoparticle film was simulated for the first time, and" unusual hot spots "were found. The "unconventional hot spot", also called "induced hot spot", induced by SPR of the "conventional hot spot" increases the concentration of hot spots, and the sensitivity of the "trimeric-silver foil/silver nanoparticle film" raman chip is about an order of magnitude higher than that of the silver colloid-raman chip, see fig. 1. Wu Shifa in 2013, in coordination with Pan Lujun, guide research institute Li Dawei published paper "J.Phys.chem.C 2013, 117, 6861-6871,Controlled Preparation ofUniform TiO 2 Catalyzed Silver Nanoparticle Films for Surface-Enhanced Raman Scattering ", a trimeric form-titanium dioxide SERS silver particle film raman chip was first developed. 201The patent (ZL 201510917332.8) of the invention of the nano metal film Raman chip with and without receptor titanium dioxide and the manufacturing method applied by the Wushi method in 5 years is authorized in 2019, and the design of the optimal parameters of the Raman chip of the trimerization type-silver foil/silver particle film Raman chip for photocatalytic growth of various titanium dioxide is disclosed for the first time, and the manufacturing method of the various Raman chips and the manufacturing method of control parameters in an industrial production line are disclosed; the optimal parameter design of the sensitivity of the Raman chip has three items: 1. quasi-contact of silver particles-i.e. gap 0.ltoreq.2 nm; 2. the optimal average diameter of the silver particles is coupled with the excitation wavelength; 3. the titanium dioxide film thickness is equal to or close to lambda/2 n or lambda/4 n.
In the process of controlling the production of the Raman spectrum chip, the quality of the same batch of products is difficult to ensure to have complete consistency by means of 'factory sampling inspection'. In order to develop the raman chip product into an industrial commodity, each raman chip commodity needs to meet the requirement of 'factory quality inspection standard', and a nondestructive quality inspection method and equipment need to be developed.
Disclosure of Invention
Aiming at the technical problems, the invention provides a nondestructive quality inspection method and equipment for a Raman chip of a silver or gold nano-particle film, which adopts an ultraviolet visible parallel light beam as a light source to obtain an extinction-absorption spectrum SPR main peak height H of the Raman chip SPR And H SPR ～H RS Calibration curve realizes' H SPR And (5) calibrating nondestructive quality inspection.
The technical scheme of the invention is as follows:
in one aspect, the invention provides a method for calibrating nondestructive quality inspection of a Raman chip of a silver or gold nanoparticle film, which comprises the following steps:
step one: selecting at least 5 calibration Raman chips with different sensitivities on a production line of the Raman chips to be detected, wherein the span of the calibration Raman chips needs to contain the whole range of qualified requirements of quality inspection standards, and the marks of the calibration Raman chips with different sensitivities in sequence adopt T, namely the photocatalysis time of the calibration Raman chips for growing silver nano particles;
step two: placing the selected calibration Raman chip in purpleIn the external visible parallel light beams, respectively collecting extinction absorption spectra, and detecting the height H of a main peak of Surface Plasmon Resonance (SPR) SPR Make scaling T-H SPR A curve;
step three: on Raman spectrometers for non-destructive quality control calibration, a calibration sample such as R6g10 is used -6 M/L, collecting Raman spectrum of the calibration Raman chip, and selecting the height H of the calibration peak RS Make scaling T-H RS A curve;
step four: according to the scaling T-H SPR And T to H RS Curve as H SPR ～H Rs A calibration curve is used for preparing a quality control limit according to the standard specification of the quality inspection sensitivity of the Raman chip;
step five: in the product quality inspection of the raman chip production line in the step one, if the peak height H of the raman chip is detected nondestructively SR And (3) if the sensitivity quality inspection formulated in the step four meets the standard, the Raman chip is qualified, otherwise, the Raman chip is unqualified.
Based on the above scheme, preferably, the raman chip is a 'trimeric type-silver foil/silver nanoparticle film' raman chip, or a gold nanoparticle film raman chip, or a gold-plated silver nanoparticle film raman chip, which is formed by photocatalytic growth of a titanium dioxide film.
Based on the scheme, the extinction absorption spectrum of the Raman chip and the height H of the SPR main peak SPR Including the sum of conventional molecular absorption, conventional elastic scattering loss, and metal Surface Plasmon Resonance (SPR) inelastic scattering extinction-absorption.
Based on the scheme, preferably, in order to prevent oxidation of the Raman chip quality inspection process in the air, H SPR Is performed in a silver nitrate solution, or in a vacuum environment, or in an inert gas, in which a silver nanoparticle film is grown.
Based on the above scheme, preferably, the scaling T-H SPR And T to H RS Curve and H SPR ～H RS Each H on the scaling curve SPR And H RS Point data, experimental average data of at least 2 scaled Raman chips with the same T value as a groupThe method comprises the steps of carrying out a first treatment on the surface of the If each H SPR And H RS The point data only adopts the experimental data of a single T value calibration Raman chip, so that the experimental data of at least 10 calibration Raman chips with different T values are needed for guaranteeing H SPR ～H RS Accuracy of the calibration curve.
On the other hand, the invention provides nondestructive quality inspection equipment used by the method, which comprises an ultraviolet visible light source, wherein a wide spectrum light beam emitted by the light source passes through a self-focusing transmission optical fiber or does not pass through the optical fiber to generate a small-caliber parallel light beam, a Raman chip to be inspected is positioned below the parallel light beam, is arranged perpendicular to the parallel light beam and is placed on a bracket, and the Raman chip is in a vacuum or inert gas environment or is placed in a silver nitrate solution for growing a silver film; the periphery of the parallel light beam and the Raman chip to be inspected is provided with a dark-phase curtain or is positioned in a dark room, the small-caliber parallel light beam which is transmitted by the Raman chip is connected to a spectrometer system through another self-focusing transmission optical fiber or not through the optical fiber, and the extinction absorption spectrum of the Raman chip to be inspected is received and recorded, and the Raman chip to be inspected is connected with a computer and H SPR ～H RS The scaling software system and the management system are responsible for processing the SPR main peak height H SPR And whether the sensitivity quality of the Raman chip in the quality inspection meets the requirements of factory quality inspection standards is displayed.
The principle of the silver or gold nanoparticle film Raman chip calibration nondestructive quality inspection method and equipment is based on the fact that in the Raman chip extinction-absorption effect, the sum of three items including conventional molecular absorption, conventional elastic scattering loss and metal Surface Plasmon Resonance (SPR) inelastic scattering extinction-absorption is included, wherein local surface plasmon resonance-SPR absorption components generated by ordered metal nano pore structures of the Raman chip are contained, otherwise, extinction absorption cannot be achieved.
Advantageous effects
The invention provides a nondestructive quality inspection method and equipment for a Raman chip of a silver or gold nanoparticle film, which adopts ultraviolet visible parallel light beams as light sources to extinction absorption spectrum SPR main peak height H SPR And H SPR ～H RS Scaling relation, realizing 'H' of the Raman chip SPR And (5) calibrating nondestructive quality inspection.
Drawings
Fig. 1 shows that in the raman chip simulation of the structure of the "trimer type-silver foil/silver nanoparticle film", the phenomenon of inducing "unconventional hot spots" is found, the hot spot density is doubled, and the raman spectrum enhancement can be about an order of magnitude higher than the sensitivity of the colloidal silver raman chip.
FIG. 2 shows the extinction-absorption spectrum H of a Raman chip SPR Schematic diagram of nondestructive quality inspection equipment;
wherein, 1-ultraviolet visible light source; a 2-spectrometer system; 3-computer and H SPR ～H RS Scaling software and a control system; 4-small-caliber self-focusing transmission optical fiber; 5-parallel light beams; 6-Raman chip schematic diagram; 7-silver nitrate aqueous solution for growing silver particle film, isolating oxygen in air, because the Raman chip is used for detecting H SPR In the process, the silver nanoparticle film is extremely easy to oxidize and damage due to irradiation of ultraviolet and visible light beams; 8-a bracket; 9-dark-phase curtains or darkrooms.
FIG. 3 is a set of atomic force microscope images, detection H, of T (2 min, 8min, 16min, 30min, and 55 min) 5 photocatalytic times "trimer-silver foil/silver nanoparticle film Raman chip SPR And H RS Scaling data schematic:
FIG. A is an atomic force microscope image of 5 different photocatalytic times "trimer-silver foil/silver particle film Raman chip";
FIG. B shows extinction-absorption spectra and SPR main peak height H of 5 different photocatalytic times "trimer-silver foil/silver particle film Raman chip SPR ；
FIG. C is a sample R6g10 of a calibration of 5 different photocatalytic times "trimer type-silver foil/silver particle film Raman chip - 6 M/L Raman spectrum and H RS 。
FIG. 4 shows calibration scaling T-H of a trimerization-silver foil/silver nanoparticle film Raman chip under the condition of growing silver nitrate solution of a silver film SPR And T to H RS Curve, and make H SPR ～H RS Calibration curveSchematic diagram, wherein the dashed line represents the known trend of the curve.
Detailed Description
The Raman chip used in the embodiment is a 'trimerization type-silver foil/silver nanoparticle film Raman chip', and the characteristics and specific preparation method can be referred to as J.Phys.chem.C 2013, 117, 68616871,Controlled Preparation ofUniform TiO 2 Catalyzed Silver Nanoparticle Films for Surface-Enhanced Raman Scattering "and invention patent (ZL 201510917332.8).
A Raman chip calibration nondestructive quality inspection method for silver or gold nanoparticle films specifically comprises the following steps:
first, according to H SPR ～H RS The calibration method requires configuration of H dedicated to the Raman chip SPR Deep refrigeration CCD Raman spectrometer for calibration and nondestructive quality inspection, and Raman spectrum standard sample-R6 g-10 with standard concentration for calibration and nondestructive quality inspection -6 M/L；
The second step is H SPR The calibration nondestructive quality inspection equipment needs to purchase three components of an ultraviolet visible wide spectrum light source, a high-sensitivity spectrometer and a notebook computer, and is designed into H in discrete or integrated manufacture as shown in figure 2 SPR ～H Rs Scaling the special equipment for nondestructive quality inspection;
third, selecting the calibration T-H on the production line of the Raman chip SPR And T to H RS Curve sum H SPR ～H RS A calibration Raman chip for calibrating the curve;
fourthly, the sensitivity of the calibration Raman chip needs to be properly equally divided, at least five different sensitivities are adopted, and the sensitivity quality of the calibration Raman chip accords with the whole range of the quality control standard; to ensure H SPR ～H RS Precision of calibration curve, 5H in each curve SPR And H RS Data, the average value of 2 experimental values of a calibration Raman chip with the same marking sensitivity is needed; if H in the curve SPR And H RS The data are all experimental values of single calibration Raman chips, so that the number of the calibration Raman chips with different sensitivities needs to be increased to not less than 10, namely H SPR ～H RS H in calibration curve SPR And H RS The experimental values of the data are not less than 10.
Fifth, different sensitivities of the raman chip are marked with different photocatalytic times T: such as 2min, 8min, 16min, 30min, and 55min, shown in figure 3-A; detection of extinction-absorption Spectrum and H of 5 calibration Raman chips SPR See fig. 3-B;
step six, respectively dripping R6g standard concentration sample on 5 calibration Raman chips, and detecting H RS See fig. 3-C;
seventh step, in the H SPR Processing T-H on notebook computer of nondestructive quality inspection equipment RS And T to H RS Curve data, create H SPR ～H RS Calibration curves, see FIGS. 4-A,4-B,4-C, respectively;
and eighth step, making a quality control range of a factory quality inspection standard-SPR peak height. After the calibration is finished, the method can be used for nondestructive delivery quality inspection of the Raman chip, ensures that each commodity delivered meets delivery standards, for example, the quality control limit is 1.5-2.4 according to the figure 4-C, and the Raman chip products on the same production line with the calibrated Raman chip are selected for detection, and when the Raman chip is H SPR When the temperature is between 1.5 and 2.4, the factory standard is met, and when the temperature is not in the section, the factory quality inspection standard is not met.
Claims (5)
1. A Raman chip calibration nondestructive quality inspection method for silver or gold nanoparticle films is characterized by comprising the following steps:
step one: selecting at least 5 calibration Raman chip sets with different sensitivities on a production line of Raman chips to be inspected, wherein the span of the calibration Raman chip sets needs to contain the whole range of qualified quality inspection standards, and the calibration Raman chips with different sensitivities are marked as T, namely the photocatalysis time of the calibration Raman chips for growing silver nano particles;
step two: respectively placing the selected calibration Raman chip sets in ultraviolet visible parallel beams, collecting extinction absorption spectrum, and detecting the height H of a main peak of Surface Plasmon Resonance (SPR) SPR Make scaling T-H SPR A curve;
step three: on a Raman spectrometer for nondestructive quality testing and calibration, a calibration sample is adopted to collect Raman spectra of the calibration Raman chip, and the height H of a calibration peak is selected RS Make scaling T-H RS A curve;
step four: according to the scaling T-H SPR And T to H RS Curve as H SPR ～H RS A calibration curve is used for preparing a quality control limit according to the standard specification of the quality inspection sensitivity of the Raman chip;
step five: in the product quality inspection of the raman chip production line in the first step, if the peak height H of the raman chip is detected in a nondestructive manner SRP In the range of the quality control limit of the quality inspection sensitivity formulated in the step four, the quality inspection of the Raman chip is qualified, otherwise, the Raman chip is unqualified;
the nondestructive quality inspection equipment used by the method comprises an ultraviolet visible light source (1), wherein a wide spectrum light beam emitted by the ultraviolet visible light source (1) passes through or does not pass through a self-focusing transmission optical fiber (4) to generate a small-caliber parallel light beam (5), a Raman chip (6) to be inspected is positioned below the parallel light beam (5) and is perpendicular to the parallel light beam, the Raman chip is arranged on a bracket (8), and the Raman chip (6) is positioned in a silver nitrate solution (7) for growing a silver nanoparticle film or in a vacuum or inert gas environment; the periphery of the parallel light beam (5) and the Raman chip (6) to be inspected is provided with a dark-phase curtain (9) or is positioned in a darkroom, the small-caliber parallel light beam is transmitted by the Raman chip (6), and is connected to the spectrometer system (2) through another self-focusing transmission optical fiber (4) or not through the optical fiber, and the extinction absorption spectrum of the Raman chip (6) is received and recorded, and a computer and H SPR ～H RS The scaling software system and the management system (3) are responsible for processing the SPR main peak height H SPR And whether the sensitivity quality of the Raman chip in the quality inspection meets the requirements of factory quality inspection standards is displayed.
2. The raman chip calibration nondestructive quality inspection method according to claim 1, wherein the raman chip is a 'trimer type-silver foil/silver nanoparticle film' raman chip, or a gold nanoparticle film raman chip, or a gold-plated silver nanoparticle film raman chip, which is grown by titanium dioxide film photocatalysis.
3. The raman chip calibration nondestructive testing method according to claim 1, wherein the extinction absorption spectrum of the raman chip and the height H of the SPR main peak SPR Including the sum of conventional molecular absorption, conventional elastic scattering loss, and metal Surface Plasmon Resonance (SPR) inelastic scattering extinction-absorption.
4. The method for Raman chip scale non-destructive quality testing according to claim 1, wherein to prevent oxidation of Raman chip quality testing process in air, H SPR The detection setting of (2) is completed in silver nitrate solution for growing silver nano particle film, or in vacuum environment, or in inert gas.
5. The raman chip scaled nondestructive testing method according to claim 1, wherein said scaled T-H SPR And T to H RS Curve and H SPR ～H RS Each H on the scaling curve SPR And H RS The point data adopts experimental average value data of a calibration Raman chip with at least 2 identical T values as a group; if each H SPR And H RS The point data only adopts the experimental data of a single T value calibration Raman chip, so that the experimental data of at least 10 calibration Raman chips with different T values are needed for guaranteeing H SPR ～H RS Accuracy of the calibration curve.
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