CN111678907A - Module for Raman detection and preparation method thereof - Google Patents
Module for Raman detection and preparation method thereof Download PDFInfo
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- CN111678907A CN111678907A CN202010552428.2A CN202010552428A CN111678907A CN 111678907 A CN111678907 A CN 111678907A CN 202010552428 A CN202010552428 A CN 202010552428A CN 111678907 A CN111678907 A CN 111678907A
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- raman
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- 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
Abstract
The invention provides a module for Raman detection and a preparation method thereof. The module comprises: a substrate; a plurality of tapered grooves provided on the substrate with a taper tip facing downward; nanoparticles collected near the cone tips of the plurality of cone-shaped grooves; and a molecule to be detected, which is arranged in the plurality of conical grooves and covers the nano particles. The invention can promote the effective aggregation of the nano particles, effectively save the use amount of the nano particles, save the cost of raw materials and effectively improve the sensitivity and the repeatability of Raman detection.
Description
Technical Field
The invention relates to the field of Raman detection, in particular to a module for Raman detection and a preparation method thereof.
Background
The Surface Enhanced Raman Scattering (SERS) technology has been receiving attention due to its high sensitivity and high detection speed, and can provide a fingerprint spectrum. The more common reinforcing substrates in the detection process are nanoparticles and liquid nanosols. The distribution of the substrates is closely related to the sensitivity and repeatability of the detection. Therefore, the aggregation of the nano particles and the distribution of multiple points in a repeatable manner are realized, and the Raman detection effect can be effectively improved.
When the enhanced substrate is a nanoparticle, the dispersion degree of the nanoparticle in the liquid is often uncontrollable after the titration of the liquid sol and in the drying process, which causes poor dispersion uniformity of the prepared nanoparticle, resulting in large relative error of the raman intensity of the same sample and waste of the substrate raw material.
When the enhanced substrate is liquid nanosol, the corresponding traditional liquid Raman detection is generally carried out in a capillary glass tube, and the problems of difficult Raman laser focusing and long time consumption exist.
In the existing research in the industry, there is also a raman detection tool using a cylindrical groove array, which is improved in the aggregation degree of nanoparticles, but still has the disadvantages of low aggregation degree, insufficient saving of nanoparticles, low enhancement effect, and the like.
Therefore, how to provide a module for performing raman detection and a method for preparing the same to effectively aggregate nanoparticles, save the usage amount of the nanoparticles, improve the sensitivity and repeatability of raman detection, and reduce the cost of raw materials has become a technical problem to be solved in the industry.
Disclosure of Invention
In view of the above problems of the prior art, the present invention provides a module for raman detection, the module comprising: a substrate; a plurality of tapered grooves provided on the substrate with a taper tip facing downward; nanoparticles collected near the cone tips of the plurality of cone-shaped grooves; and a molecule to be detected, which is arranged in the plurality of conical grooves and covers the nano particles.
In one embodiment, the substrate is made of silica glass, the substrate is a rectangular parallelepiped, the length of the rectangular parallelepiped is 7.5 cm, the width of the rectangular parallelepiped is 2.5 cm, and the height of the rectangular parallelepiped is 1 cm.
In one embodiment, the plurality of tapered grooves include a plurality of conical grooves arranged in an array, the conical grooves have a height of not less than 2 mm and a diameter of a bottom surface of not less than 2 mm.
In one embodiment, the walls of the plurality of tapered grooves are covered with a raman-enhanced metal film, and the nanoparticles are raman-enhanced metal nanoparticles collected on the raman-enhanced metal film.
In one embodiment, the raman-enhancing metal comprises gold, silver and copper having raman-enhancing effect.
The invention also provides a method for preparing a module for raman detection according to any one of the preceding claims, comprising the following steps: (a) providing a substrate provided with a plurality of conical grooves; (b) carrying out one or more times of titration of a preset amount of nano hydrosol in the plurality of conical grooves, and carrying out drying and curing after each titration, wherein the nano hydrosol contains nano particles which are gathered near the conical tips of the plurality of conical grooves in a preset distribution after final drying and curing; and (c) titrating the solution to be detected in the plurality of conical grooves and drying the solution to be detected so that the molecules to be detected corresponding to the solution to be detected are covered on the nano particles and are suitable for Raman detection.
The preparation method also comprises the following steps between the steps (a) and (b): (a0) applying a Raman enhanced metal film on sidewalls of the plurality of tapered recesses.
In one embodiment, the nanoparticles collected near the tips of the plurality of tapered recesses in step (b) are raman-enhanced metal nanoparticles collected on the raman-enhanced metal film.
In one embodiment, the raman-enhancing metal comprises gold, silver and copper having raman-enhancing effect.
The invention also provides a preparation method of the module for Raman detection, which comprises the following steps: (a1) providing a substrate provided with a plurality of conical grooves; (b1) mixing the liquid sol containing the nano particles with a solution to be detected containing molecules to be detected to form mixed liquid sol; (c1) titrating the mixed solution sol into the plurality of conical grooves; and (d1), standing to enable the nano particles to gather near the conical tips of the conical grooves, and enabling the molecules to be detected to cover the nano particles so as to be suitable for liquid Raman detection.
Compared with the prior art, the invention has the following beneficial effects:
first, the plurality of tapered grooves in the present invention are disposed on the substrate in a manner that the tapered tips face downward, so that the nanoparticles are collected near the tapered tips of the plurality of tapered grooves, and the tapered grooves can effectively improve the collection degree of the nanoparticles, prevent dispersion, and improve the spectral detection sensitivity.
Secondly, in the prior art, the cylindrical grooves cannot effectively gather the nano particles, so that the nano particles are freely dispersed, and the enhancement effect of the Raman test is lowered; according to the invention, under the condition of less nano particles, through the plurality of conical grooves, the nano particles can obtain stronger Raman detection signals no matter how large the form and size of the nano particles.
Thirdly, the plurality of tapered grooves of the present invention include a plurality of tapered grooves arranged in an array manner, so that the detection can be repeated, the detection stability is improved, and the material and cost can be effectively saved.
Fourthly, the side surface of the conical groove can be covered with a layer of Raman enhancement metal film if necessary, so that the Raman detection signal, the Raman detection intensity and the detection sensitivity are further improved.
Drawings
The above features and advantages of the present disclosure will be better understood upon reading the detailed description of embodiments of the disclosure in conjunction with the following drawings. In the drawings, components are not necessarily drawn to scale, and components having similar relative characteristics or features may have the same or similar reference numerals.
Fig. 1 is a schematic structural diagram of a module for raman detection according to the present invention.
Fig. 2 is a schematic diagram of a specific structure of the tapered groove in fig. 1.
FIG. 3 is a schematic diagram of Raman detection using the module of FIG. 1.
Fig. 4 is a graph showing the variation of electric field around gold/silver nanoparticles on a substrate at different inter-particle distances.
FIG. 5 is a schematic illustration of the degree of particle agglomeration in a conical recess of the present invention compared to a prior art cylindrical recess.
Fig. 6 is a flowchart of a first embodiment of a method of manufacturing a module for performing raman detection according to the present invention.
Fig. 7 is a flowchart of a second embodiment of a method of manufacturing a module for performing raman detection according to the present invention.
Detailed description of the preferred embodiments
The invention will be described in detail below with reference to the accompanying drawings and specific embodiments so that the objects, features and advantages of the invention can be more clearly understood. It should be understood that the aspects described below in connection with the figures and the specific embodiments are exemplary only, and should not be construed as limiting the scope of the invention in any way. The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise.
Referring to fig. 1 in combination with fig. 2, fig. 1 shows a schematic structural diagram of the module for performing raman detection according to the present invention. As shown in fig. 1, the module includes a substrate 1, a plurality of tapered grooves 10, nanoparticles (also referred to as "solid nanoparticles") 2, a molecule to be measured 3, and a raman-enhanced metal film 4, wherein the raman-enhanced metal film 4 is optional. The various components of the module will be described in detail below.
The material of the substrate 1 may be silica glass, or other glass or other materials commonly used in the art. In one embodiment, the substrate 1 is a rectangular parallelepiped with a length of 7.5 cm, a width of 2.5 cm, and a height of 1 cm. In other embodiments, the substrate 1 may have other shapes suitable for raman detection, such as a cube, a cuboid-like shape, or a cube-like shape, and the size of the substrate 1 may be a size suitable for raman detection other than the above parameters.
A plurality of toper recesses 10 set up with the awl point mode down on base plate 1, a plurality of toper recesses are convenient for repeat and are detected, improve and detect stability. The plurality of tapered recesses 10 may be arranged on the substrate 1 in an array, as shown in fig. 1, and may be arranged in a matrix of 2 rows and 7 columns (2 × 7), or may be arranged in other matrices as the case may be. The plurality of tapered grooves 10 includes a plurality of conical grooves 10 arranged in an array, and the height of the conical grooves 10 is not less than 2 millimeters (mm), and the diameter of the bottom surface thereof is not less than 2 mm. In one embodiment, the height of the conical recess 10 may be 3 mm, and the diameter of the bottom surface thereof may be 5 mm.
The size of the conical recess 10 is preferably such that it is visible to the naked eye, which conical recess 10 does not put too high demands on the manufacturing process (e.g. laser grooving) on the one hand, so that the manufacturing costs can be reduced; on the other hand, the titration of the tapered recesses 10 can be performed directly by the naked eye without any aid of any magnifying aids.
As shown in fig. 2, the nanoparticles 2 are collected near the tapered tips of the plurality of tapered recesses 10. The nanoparticles 2 may have a particle diameter of several nanometers or several tens of nanometers, and may be raman-enhanced metal nanoparticles such as gold nanoparticles, silver nanoparticles, or copper nanoparticles. The Raman-enhanced metal nanoparticles can also be metal oxides with Raman enhancement effect, such as TiO, commonly used in the industry2And the like.
The molecules 3 to be tested are arranged in the conical grooves 10 and cover the nanoparticles 2, and the molecules 3 to be tested are gathered near the conical tips of the conical grooves 10 along the stacking shape of the nanoparticles 2.
Optionally, theThe walls of the plurality of tapered grooves 10 can be covered with raman-enhanced metal films 4 for improving raman detection intensity and detection sensitivity, the raman-enhanced metal films 4 include gold films, silver films, copper films and the like, and the corresponding raman-enhanced metal nanoparticles 2 are gathered on the raman-enhanced metal films 4. The raman-enhanced metal film 4 may also be a metal oxide film having a raman enhancement effect, such as TiO, which is commonly used in the art2Films, and the like.
Referring to fig. 3, a schematic diagram of raman detection using the module of fig. 1 is shown. The laser 5 can be lasers with various wavelengths such as 514nm, 532nm, 633nm or 785 nm; the wavelength of the laser 6 can be 514nm, 532nm, 633nm or 785 nm. During Raman detection, the laser 6 with a preset wavelength is generated by the laser 5, the laser 6 irradiates the molecule 3 to be detected, and the molecule 3 to be detected covers the nano-particle 2 to generate enhanced Raman scattering. Scattered light corresponding to the Raman scattering can reach a detector through a series of optical path elements, and a corresponding Raman spectrum is obtained through computer processing.
Referring to fig. 4, a graph showing the variation of electric field around gold/silver (Au/Ag) nanoparticles on a substrate at different inter-particle distances is shown. As shown in fig. 4, the smaller the distance between the nanoparticles 2 such as Au/Ag particles on the substrate 11, the more significant the electric field variation around the Au/Ag particles, i.e. the larger the value of E/E0, the more significant the corresponding raman signal enhancement, and the tapered grooves of the present invention can effectively reduce the spacing between the nanoparticles, thereby obtaining the enhanced raman signal.
Figure 5 shows a comparison of the degree of particle agglomeration in a conical recess of the present invention with a cylindrical recess of the prior art. As shown in the left diagram of fig. 5, no matter how many nanoparticles are in the tapered groove 10, the nanoparticles can be gathered at the tapered tip of the tapered groove 10, so that the distance between the nanoparticles is as small as possible, and it can be known from fig. 4 and the above description that the higher the aggregation degree of the nanoparticles, the more obvious the raman enhancement effect is; in contrast, when the number of nanoparticles is small, the nanoparticles can only be sparsely dispersed on the bottom of the cylindrical groove, and a strong raman signal enhancement cannot be formed in the cylindrical groove of the prior art shown in the right diagram of fig. 4.
Referring to fig. 6, a flow chart of a first embodiment of a method of fabricating a module for raman detection of the present invention is shown. As shown in fig. 6, the method S60 for manufacturing a module for raman detection first performs step S600 of providing a substrate having a plurality of tapered grooves formed thereon. The substrate may be a substrate 1 having a plurality of tapered recesses 10 disposed thereon as shown in fig. 1, the specific configuration and parameters of which may be understood with reference to fig. 1 and the description thereof above.
The preparation method S60 proceeds to step S620, and a raman-enhanced metal film is applied on the sidewalls of the plurality of tapered recesses. The raman-enhanced metal film in step S620 includes a gold film, a silver film, a copper film, and the like, which can improve raman detection intensity and detection sensitivity.
The preparation method S60 continues with step S640 of performing one or more titrations of a predetermined amount of nano-hydrosol in the plurality of tapered grooves, and performing drying and curing after each titration, wherein the nano-hydrosol contains nano-particles, and the nano-particles are gathered in a predetermined distribution near the tapered tips of the plurality of tapered grooves after final drying and curing. In the step S640, each time the nano-sized hydrosol is titrated and dried, the nano-sized particles are gathered at the cone tip of the tapered groove and are not dispersed and distributed; the titration of the nanosilux may be repeated until a satisfactory dense distribution of nanoparticles is achieved.
In one embodiment, the nanoparticles collected near the conical tips of the plurality of conical grooves are raman-enhanced metal nanoparticles directly collected on the raman-enhanced metal film, and the raman-enhanced metal is gold or silver or copper or metal oxide or the like having a raman enhancement effect.
The preparation method S60 then proceeds to step S660, where a solution to be detected is titrated in the plurality of tapered grooves and dried, so that the molecules to be detected corresponding to the solution to be detected are covered on the nanoparticles and are suitable for raman detection.
It should be noted that step S620 in fig. 6 is not necessary, and in some embodiments of the method for preparing the module for raman detection, step S620 may not be included; however, the step S620 of applying the raman-enhanced metal film on the sidewalls of the plurality of tapered recesses can further improve the raman intensity and the detection sensitivity due to the dual enhancement of the raman-enhanced metal film and the nanoparticles, compared to the case of not applying the raman-enhanced metal film.
Referring to fig. 7, a flow chart of a second embodiment of a method of making a module for performing raman detection of the present invention is shown. Unlike the first embodiment of fig. 6, in which the module for raman detection is a solid sol, the second embodiment of fig. 7 is a liquid sol or a liquid sol. As shown in fig. 7, the method S70 for manufacturing a module for raman detection first performs step S700 of providing a substrate having a plurality of tapered grooves formed thereon. The substrate may also be a substrate 1 having a plurality of tapered recesses 10 disposed thereon as shown in fig. 1.
The preparation method S70 proceeds to step S720, and a raman-enhanced metal film is applied on the sidewalls of the plurality of tapered grooves. The raman enhanced metal film in step S720 also includes a gold film, a silver film, a copper film, a metal oxide film, or the like having a raman enhancing effect, which can improve raman detection intensity and detection sensitivity.
The preparation method S70 proceeds to step S740, and mixes the liquid sol containing the nanoparticles with the solution to be detected containing the molecule to be detected, thereby forming a mixed liquid sol. In an embodiment, the nanoparticles are raman-enhanced metal nanoparticles such as silver nanoparticles or gold nanoparticles or copper nanoparticles.
Preparation method S70 then proceeds to step S760, where the mixed liquid sol is titrated into the plurality of tapered recesses.
The preparation method S70 then proceeds to step S780, and stands to make the nanoparticles gather near the conical tips of the plurality of conical grooves, and the molecules to be detected are covered on the nanoparticles to be suitable for liquid raman detection. The standing time can be determined according to specific conditions.
When the adsorption force of the molecule to be detected is strong, the molecule to be detected starts to be adsorbed on the nanoparticles in the mixed solution sol formed in step S740, and the nanoparticles and the molecule to be detected adsorbed thereon are precipitated and aggregated near the cone tip in the standing process of step S780.
When the adsorption force of the molecule to be detected is weak, the molecule to be detected is not combined before the standing process of step S780, and in the standing process, because the nanoparticles are heavier than the molecule to be detected, the nanoparticles are firstly gathered near the cone tip of the cone-shaped groove, and the molecule to be detected is covered on the nanoparticles later.
Similar to step S620 in the preparation method S60 in fig. 6, step S720 in the preparation method S70 in fig. 7 is also optional, and the raman detection intensity and detection sensitivity of the method S70 with step S720 are higher than those of the method S70 without step S720.
The module for Raman detection comprises a substrate, a plurality of conical grooves arranged on the substrate in a mode that conical tips face downwards, nanoparticles gathered near the conical tips of the conical grooves, and molecules to be detected, wherein the molecules to be detected are arranged in the conical grooves and cover the nanoparticles. The invention can promote the effective aggregation of the nano particles, save the use amount of the nano particles, effectively save the cost of raw materials and improve the sensitivity and the repeatability of Raman detection.
The embodiments described above are provided to enable persons skilled in the art to make or use the invention and that modifications or variations can be made to the embodiments described above by persons skilled in the art without departing from the inventive concept of the present invention, so that the scope of protection of the present invention is not limited by the embodiments described above but should be accorded the widest scope consistent with the innovative features set forth in the claims.
Claims (10)
1. A module for raman detection, the module comprising:
a substrate;
a plurality of tapered grooves provided on the substrate with a taper tip facing downward;
nanoparticles collected near the cone tips of the plurality of cone-shaped grooves; and
and the molecules to be detected are arranged in the plurality of conical grooves and cover the nanoparticles.
2. The module of claim 1, wherein the substrate is made of silica glass; the substrate is a cuboid, the length of the substrate is 7.5 cm, the width of the substrate is 2.5 cm, and the height of the substrate is 1 cm.
3. The module of claim 1, wherein the plurality of tapered grooves comprise a plurality of conical grooves arranged in an array, the conical grooves having a height of not less than 2 mm and a diameter of at least 2 mm.
4. The module of claim 1, wherein walls of the plurality of tapered recesses are covered with a Raman enhanced metal film, the nanoparticles are Raman enhanced metal nanoparticles, and the Raman enhanced metal nanoparticles are collected on the Raman enhanced metal film.
5. The module for raman detection according to claim 4, wherein said raman enhancing metal comprises gold, silver and copper having raman enhancing effect.
6. A method of preparing a module for Raman detection according to any one of claims 1 to 5, comprising the steps of:
(a) providing a substrate provided with a plurality of conical grooves;
(b) carrying out one or more times of titration of a preset amount of nano hydrosol in the plurality of conical grooves, and carrying out drying and curing after each titration, wherein the nano hydrosol contains nano particles which are gathered near the conical tips of the plurality of conical grooves in a preset distribution after final drying and curing; and
(c) titrating the solution to be detected in the plurality of conical grooves and drying the solution to be detected so that the molecules to be detected corresponding to the solution to be detected are covered on the nano particles and are suitable for Raman detection.
7. The method of claim 6, further comprising, between steps (a) and (b), the steps of: (a0) applying a Raman enhanced metal film on sidewalls of the plurality of tapered recesses.
8. The method of claim 7, wherein the nanoparticles collected near the tips of the plurality of tapered recesses in step (b) are Raman-enhanced metal nanoparticles collected on the Raman-enhanced metal film.
9. The method of claim 7, wherein the Raman-enhanced metal comprises gold, silver, and copper having a Raman-enhancing effect.
10. A method of preparing a module for Raman detection according to any one of claims 1 to 5, comprising the steps of:
(a1) providing a substrate provided with a plurality of conical grooves;
(b1) mixing the liquid sol containing the nano particles with a solution to be detected containing molecules to be detected to form mixed liquid sol;
(c1) titrating the mixed solution sol into the plurality of conical grooves; and
(d1) and standing to enable the nano particles to be gathered near the conical tips of the plurality of conical grooves, wherein the molecules to be detected are covered on the nano particles so as to be suitable for liquid Raman detection.
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| CN110044872A (en) * | 2019-05-10 | 2019-07-23 | 山东大学 | A kind of surface enhanced Raman substrate and the preparation method and application thereof |
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2020
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| US20050211566A1 (en) * | 2004-03-23 | 2005-09-29 | Fuji Photo Film Co., Ltd. | Fine structural body and method of producing the same |
| CN107567579A (en) * | 2015-07-20 | 2018-01-09 | 惠普发展公司，有限责任合伙企业 | Structure for SERS |
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