CN113406055B - Preparation method of secondary reduced tin-silver dendrite nanostructure for enhancing Raman spectrum - Google Patents
Preparation method of secondary reduced tin-silver dendrite nanostructure for enhancing Raman spectrum Download PDFInfo
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Abstract
The application relates to a preparation method of a secondary reduced tin-silver dendrite nanostructure for enhancing Raman spectrum, and particularly relates to the field of preparation of dendrite nanostructures. The application provides a preparation method, place predetermined substrate and react first default time in stannous chloride-ethanol solution, obtain tin dendrite nanostructure, under the light-resistant condition, place tin dendrite nanostructure and react the second default time in silver nitrate solution, obtain tin silver dendrite nanostructure, will predetermine probe molecule deposit on tin silver dendrite nanostructure's surface, step and the step of one step of deposit through two steps replacement reaction, preparation obtains tin silver dendrite nanostructure, and through the surface deposit probe molecule at tin silver dendrite nanostructure, under the exciting light incidence condition, because tin silver dendrite nanostructure is to different probe molecules, different scattering spectra have, tin silver dendrite nanostructure surveys through the scattering intensity that increases probe molecule, through the intensity that increases the scattering peak promptly, realize the reinforcing to the raman spectrum.
Description
Technical Field
The application relates to the field of dendritic crystal nanostructure preparation, in particular to a preparation method of a secondary reduced tin-silver dendritic crystal nanostructure for enhancing Raman spectrum.
Background
Since the discovery of surface enhanced Raman Scattering Effect (SERS) in 1970, non-contact, non-destructive Raman Spectroscopy techniques with detection of Single-molecule limiting analytes have shown great viability and have been used in a number of fieldsDomains are receiving a wide range of attention. Because the Raman spectrum frequency shift only depends on the vibration energy level of the target molecule and is irrelevant to the excitation wavelength, the Raman spectrum can be used as the fingerprint spectrum of the molecule, the target identification is extremely strong, and therefore, in the practical engineering application, the Raman spectrum technology receives more and more attention. The Raman scattering cross section of the molecule is small and is usually 10 -30 –10 -25 In the range of cm2, the Raman signal of the free-state molecule is very weak, and the requirement of the spectral behavior of the detector on the test environment is very strict, so that the engineering popularization is greatly limited.
To further enhance the raman scattering spectroscopic signal, the investigator adsorbs the detected molecule to the surface of the noble metal nanostructure and observes an enhancement in raman spectroscopic intensity. In the dendritic metal nano structure, strong local field coupling can occur between two adjacent dendritic crystals, so that an electromagnetic hot point is easy to form, the electron radiation transition rate of molecules can be effectively enhanced, and the Raman spectrum enhancement is realized. Therefore, it is particularly important to prepare a metal dendrite nanostructure substrate having low cost and high stability.
However, the general preparation process of the metal dendrite nanostructure in the prior art is complex, has high cost and is difficult to be applied to the enhanced Raman scattering spectrum.
Disclosure of Invention
The invention aims to provide a preparation method of a secondary reduced tin-silver dendrite nanostructure for enhancing Raman spectroscopy, aiming at overcoming the defects in the prior art, so as to solve the problems that the general preparation process of the metal dendrite nanostructure in the prior art is complex, the cost is high, and the metal dendrite nanostructure is difficult to apply to enhancing Raman scattering spectroscopy.
In order to achieve the above purpose, the embodiment of the present invention adopts the following technical solutions:
in a first aspect, the present application provides a method for preparing a secondary reduced tin-silver dendrite nanostructure for enhanced raman spectroscopy, the method comprising:
placing a preset substrate in a stannous chloride-ethanol solution for reacting for a first preset time to obtain a tin dendrite nano structure;
placing the tin dendrite nano structure in a silver nitrate solution to react for a second preset time under a dark condition to obtain a tin-silver dendrite nano structure;
and depositing preset probe molecules on the surface of the tin-silver dendrite nanostructure.
Optionally, the first predetermined time is 1 minute to 5 minutes, and the second predetermined time is 30 minutes to 180 minutes.
Optionally, the step of placing the predetermined substrate in a stannous chloride-ethanol solution for a first predetermined time to obtain the tin dendrite nanostructure further includes:
SnCl 2 ·2H 2 Dissolving the O crystal in ethanol to obtain a stannous chloride-ethanol solution;
and grinding, polishing and cleaning the surface of the preset substrate by using a preset method.
Optionally, the SnCl 2 ·2H 2 The amount of O crystal is 0.034g, the amount of ethanol is 30ml, and the concentration of stannous chloride-ethanol solution is 0.5X 10 -2 mol/L。
Optionally, the step of placing the tin dendrite nanostructure in a silver nitrate solution for a second preset time under a dark condition to obtain a tin-silver dendrite nanostructure further includes:
blowing the tin dendrite nanostructure with nitrogen;
and putting the silver nitrate crystal solution in deionized water to obtain a silver nitrate solution.
Alternatively, the amount of the deionized water is 100ml, the amount of the silver nitrate crystals is 0.17g, and the concentration of the silver nitrate solution is 0.01mol/L.
Optionally, the probe molecule is crystal violet.
The invention has the beneficial effects that:
the application provides a preparation method of secondary reduction tin silver dendrite nanostructure of enhanced Raman spectroscopy, to predetermine the substrate and place the first time of predetermineeing of reaction in stannous chloride-ethanol solution, obtain tin dendrite nanostructure, under the light-resistant condition, place tin dendrite nanostructure and react the second time of predetermineeing in silver nitrate solution, obtain tin silver dendrite nanostructure, to predetermine probe molecule deposit on tin silver dendrite nanostructure's surface, this application is through the step of two-step replacement reaction and the step of one step of deposit, preparation has obtained tin silver dendrite nanostructure, and through the surface deposition probe molecule at this tin silver dendrite nanostructure, under excitation light incident condition, because this tin silver dendrite nanostructure is to different probe molecules, different scattering spectra have, this tin silver dendrite nanostructure is through the optical radiation efficiency who increases probe molecule, through the intensity that increases the scattering peak promptly, realize the reinforcing to Raman spectroscopy.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic flow chart illustrating a method for preparing a secondary reduced tin-silver dendrite nanostructure for enhancing raman spectroscopy according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of another method for fabricating secondary reduced tin-silver dendrite nanostructures for enhanced Raman spectroscopy according to an embodiment of the present invention;
FIG. 3 is a schematic flow chart of another method for fabricating secondary reduced tin-silver dendrite nanostructures for enhanced Raman spectroscopy according to an embodiment of the present invention;
fig. 4 is a structural diagram of a secondary reduced tin-silver dendrite nanostructure for enhancing raman spectroscopy according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are one embodiment of the present invention, and not all embodiments. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Note that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
In order to make the implementation of the present invention clearer, the following detailed description is made with reference to the accompanying drawings.
FIG. 1 is a schematic flow chart of a method for preparing a secondary reduced tin-silver dendrite nanostructure for enhanced Raman spectroscopy according to an embodiment of the present invention; as shown in fig. 1, the present application provides a method for preparing a secondary reduced tin-silver dendrite nanostructure for enhancing raman spectroscopy, the method comprising:
s101, placing the preset substrate in a stannous chloride-ethanol solution to react for a first preset time to obtain the tin dendrite nano structure.
The preset substrate is used for bearing the structure prepared in the present application, the preset substrate may be aluminum or other metal materials, and is not specifically limited herein, for convenience of description, the preset substrate is described herein as metal aluminum, the preset substrate made of metal aluminum is generally shaped as an aluminum foil, the size of the preset substrate is determined according to actual needs, and is not specifically limited herein, the preset substrate is placed in a stannous chloride-ethanol solution prepared in advance, so that the preset substrate reacts in the stannous chloride-ethanol solution, since the stannous chloride-ethanol solution contains chloride ions and tin ions, and since stannous chloride is only soluble in an organic solvent and insoluble in water, the stannous chloride is dissolved in the ethanol solution in the present application to form a stannous chloride-ethanol solution, and the tin ions in the stannous chloride-ethanol solution can react with aluminum atoms in the preset substrate made of aluminum, so that replaced tin atoms are attached to the surface of the preset substrate made of aluminum, and a nano dendritic structure is formed on the surface of the preset substrate made of aluminum, that the tin atoms grow on the surface of aluminum material according to the shape of the dendritic crystal of the preset substrate.
The term explains that dendrites, i.e., dendrite crystals, are crystals that develop in a typical multi-branch tree-like form. Dendrite growth is very common and is illustrated by snow formation and frost-like patterns on the windows, the dendrites forming a natural fractal pattern.
And S102, placing the tin dendrite nano structure in a silver nitrate solution to react for a second preset time under a dark condition, so as to obtain the tin silver dendrite nano structure.
The tin dendrite nanostructure formed by a dendrite structure of a layer of tin atoms is formed on the surface of the preset substrate, the tin dendrite nanostructure is placed in a silver nitrate solution, so that the tin atoms in the tin dendrite nanostructure react with the silver nitrate solution, and because silver ions and nitric acid ions exist in the silver nitrate solution, the silver ions can replace the tin atoms in the tin dendrite nanostructure, then under the action of the silver ions, partial tin atoms on the surface of the tin dendrite nanostructure are replaced by the silver ions, so that partial tin atoms of the tin dendrite nanostructure are replaced by the silver atoms, namely the surface of the preset substrate forms the tin-silver dendrite nanostructure, namely the tin-silver dendrite nanostructure is formed on the surface of the preset substrate by using tin and silver; it should be noted that the shape, size, morphology and other geometric data of the dendrites prepared in the present application are related to the time of preparation, and are not limited in this respect.
S103, depositing preset probe molecules on the surface of the tin-silver dendrite nanostructure.
Under the condition of exciting light incidence, the tin-silver dendrite nano structure has different scattering spectra and Raman spectrum enhancement for different probe molecules. And depositing the preset probe molecules on the surface of the tin-silver dendrite nano structure by using a deposition method, namely arranging a structural layer formed by the probe molecules on the surface layer of the tin-silver dendrite nano structure on the surface of the preset substrate.
Optionally, the first predetermined time is 1 minute to 5 minutes and the second predetermined time is 30 minutes to 180 minutes.
FIG. 2 is a schematic flow chart of another method for fabricating secondary reduced tin-silver dendrite nanostructures for enhanced Raman spectroscopy according to an embodiment of the present invention; as shown in fig. 2, optionally, the step of placing the predetermined substrate in the stannous chloride-ethanol solution for a first predetermined time to obtain the tin dendrite nanostructure further includes:
s201, adding SnCl 2 ·2H 2 Dissolving the O crystal in ethanol to obtain stannous chloride-ethanol solution.
Since the SnCl2.2H2O crystal can be dissolved in organic solution, the SnCl is dissolved 2 ·2H 2 And mixing the O crystal with the ethanol solution to obtain the stannous chloride-ethanol solution, wherein the concentration and the amount of the stannous chloride-ethanol solution are determined according to actual needs and are not particularly limited herein.
S202, grinding, polishing and cleaning the surface of the preset substrate by using a preset method.
In order to facilitate the reaction between the preset substrate and the tin ions, before the reaction, the surface of the preset substrate is polished, the specific steps of polishing are determined according to actual needs, and are not specifically limited herein.
Optionally, the SnCl 2 ·2H 2 The amount of O crystal is 0.034g, the amount of ethanol is 30ml, and the concentration of stannous chloride-ethanol solution is 0.5X 10 -2 mol/L。
0.034g of SnCl 2 ·2H 2 O crystals as a solvent, 30ml of ethanol as a solution, the SnCl 2 ·2H 2 The ratio of the O crystal to the ethanol is determined according to the amount of the stannous chloride-ethanol solution required, and is not described herein.
FIG. 3 is a schematic flow chart of another method for fabricating secondary reduced tin-silver dendrite nanostructures for enhanced Raman spectroscopy according to an embodiment of the present invention; as shown in fig. 3, optionally, the step of placing the tin dendrite nanostructure in a silver nitrate solution for a second predetermined time under a dark condition to obtain the tin silver dendrite nanostructure further includes:
s301, blowing the tin dendrite nano structure by using nitrogen;
because the physical and chemical properties of nitrogen are stable, can not react with other ions of this application, use nitrogen to weather the liquid on this tin dendrite to subsequent reaction.
S302, putting the silver nitrate crystal solution into deionized water to obtain a silver nitrate solution.
Using 0.17g of silver nitrate crystal, and putting the silver nitrate crystal into 100ml of deionized water to obtain 0.01mol/L of silver nitrate solution, namely taking 0.17g of silver nitrate crystal as a solvent, and taking 100ml of deionized water as a solution, wherein the ratio of the silver nitrate crystal to the deionized water is determined according to the required amount of the silver nitrate solution, and details are not repeated herein.
Alternatively, the amount of the deionized water is 100ml, the amount of the silver nitrate crystals is 0.17g, and the concentration of the silver nitrate solution is 0.01mol/L.
Optionally, the probe molecule is any one of rhodamine and crystal violet.
The probe molecule may be rhodamine or crystal violet, and is not particularly limited herein.
Fig. 4 is a structural diagram of a structure prepared by a method for preparing a secondary reduced tin-silver dendrite nanostructure for enhancing raman spectroscopy according to an embodiment of the present invention; as shown in fig. 4, according to the preparation method of the secondary reduced tin-silver dendrite nanostructure for enhancing raman spectroscopy, since the above steps are only adopted, the tin-silver dendrite nanostructure is simply prepared, and since dendrite formation is formed according to diffusion-limited aggregation and directional attachment mechanisms, compared with other preparation methods, the preparation method of the present application has high stability, and according to experiments, the tin-silver dendrite nanostructure prepared by the preparation method of the present application has strong stability and high raman activity; in fig. 4 (a), it can be observed that at the beginning of the reaction, displaced silver atoms are deposited on the Sn dendrites, as shown by the adsorption of silver nanoparticle clusters on the surface of the Sn dendrites, forming a composite structure, with Ag particles smaller than Sn dendrites and with a particle size of about 200nm. Along with the prolonging of the reaction time, the generated silver nano structure is gradually accumulated, and dendritic crystals and fractal nano structures are generated on the surface of the Sn dendritic crystals. As shown in fig. 4 (b), the generated Ag nanoparticles accumulated on the surface of tin dendrites, and the particle size became small by about 130nm. When the reaction time was increased to 90min, ag particles on the surface of the tin dendrite aggregated to form a dendrite structure, constituting a Sn-Ag layered dendrite structure, it was observed that there was a dendrite structure in which Ag particles aggregated to form a main trunk having a size of about 5 to 8 μm and fine side branches having a size of 2 μm, as shown in FIG. 4 (c). As the reaction time increases, ag nanoparticles are accumulated on the surface of Ag dendrites, forming a complex structure having a plurality of nanogaps, as shown in fig. 4 (d). During the reaction, the Ag + concentration is reduced continuously, and the Ag nano-particles formed by replacement become smaller in size and have the diameter of 60nm and are attached to the surface of the formed dendritic nano-structure, as shown in FIG. 4 (e). In FIG. 4 (f), it can be observed that the size of the branches becomes larger with the increase of the reaction time, about 10 μm and the symmetrically distributed multi-layered nanostructure is formed, and the side branch breakage phenomenon occurs. During the reaction process, ag atoms are gradually accumulated and accumulated on the surface of Sn dendrite. And this application can be through the shape, size and the form of control reaction time control dendrite, consequently at actual operation convenience, the preparation technique of this application is simple and practical, and in practical application, the execution of this step need go on under the light-resistant condition.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing a secondary reduced tin-silver dendrite nanostructure for enhanced raman spectroscopy, the method comprising:
placing a preset substrate in a stannous chloride-ethanol solution for reacting for a first preset time to obtain a tin dendrite nano structure;
placing the tin dendrite nano structure in a silver nitrate solution to react for a second preset time under a dark condition to obtain a tin-silver dendrite nano structure;
depositing preset probe molecules on the surface of the tin-silver dendrite nanostructure;
the first preset time is 2 minutes, the second preset time is 120 minutes, and the silver nano particles are accumulated on the surface of the silver dendrite to form a complex structure with a plurality of nano gaps.
2. The method for preparing a secondary reduced tin-silver dendrite nanostructure for enhanced raman spectroscopy of claim 1, wherein the step of placing the predetermined substrate in a stannous chloride-ethanol solution for a first predetermined time to obtain the tin dendrite nanostructure further comprises:
SnCl 2 ·2H 2 Dissolving the O crystal in ethanol to obtain a stannous chloride-ethanol solution;
and grinding, polishing and cleaning the surface of the preset substrate by using a preset method.
3. The method of claim 2, wherein the SnCl is a secondary reduced tin-silver dendrite nanostructure that enhances raman spectroscopy 2 ·2H 2 The amount of O crystal is 0.034g, the amount of ethanol is 30ml, and the concentration of the stannous chloride-ethanol solution is 0.5 multiplied by 10 -2 mol/L。
4. The method for preparing a secondary reduced tin-silver dendrite nanostructure for enhancing raman spectrum according to claim 3, wherein the step of placing the tin dendrite nanostructure in silver nitrate solution for a second predetermined time under dark condition further comprises before the step of obtaining the tin-silver dendrite nanostructure:
blowing the tin dendrite nanostructure dry using nitrogen;
and putting the silver nitrate crystal solution in deionized water to obtain a silver nitrate solution.
5. The method of preparing a secondary reduced tin-silver dendrite nanostructure for enhanced raman spectroscopy of claim 4, wherein the amount of deionized water is 100ml, the amount of silver nitrate crystals is 0.17g, and the concentration of silver nitrate solution is 0.01mol/L.
6. The method for preparing secondary reduced tin-silver dendrite nanostructure for enhanced raman spectroscopy according to any one of claims 1-5, wherein the probe molecule is crystal violet.
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