CN113638035A - Porous silicon-silver nano dendrite particle, preparation method thereof and SERS detection method - Google Patents

Porous silicon-silver nano dendrite particle, preparation method thereof and SERS detection method Download PDF

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CN113638035A
CN113638035A CN202110780137.3A CN202110780137A CN113638035A CN 113638035 A CN113638035 A CN 113638035A CN 202110780137 A CN202110780137 A CN 202110780137A CN 113638035 A CN113638035 A CN 113638035A
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porous silicon
silver nano
solution
silicon
corrosion
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葛道晗
赵承祥
张立强
胡州
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Jiangsu University
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    • 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
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    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons

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Abstract

The invention relates to a porous silicon-silver nano dendrite particle and a preparation and SERS detection method thereof, which comprises the steps of selecting a silicon wafer, cleaning the silicon wafer, preparing electrolytic corrosion liquid, electrifying for corrosion, preparing electrolytic separation liquid, electrifying for separation and ultrasonically shattering, wherein firstly, acetone, alcohol and deionized water are respectively used for ultrasonically cleaning the silicon wafer so as to remove oil stains and impurities on the porous silicon; preparing electrolyte from hydrofluoric acid, dimethylformamide and silver nitrate solution according to a certain proportion; then, carrying out electrochemical anodic corrosion on the silicon wafer; then preparing electrolyte from hydrofluoric acid and ethanol solution according to a certain proportion to replace the original solution for electrochemical separation; finally, the sample is washed by deionized water and is placed into a container for ultrasonic vibration crushing. The invention provides a stepwise synthesis preparation method, which is characterized in that a porous silicon-silver nano dendritic crystal particle structure is made into a particle state for the first time, and the flexible detection of a detected substance can be realized.

Description

Porous silicon-silver nano dendrite particle, preparation method thereof and SERS detection method
Technical Field
The invention belongs to the field of electrochemical corrosion and silicon microstructure preparation, and particularly relates to porous silicon-silver nano dendrite particles, preparation thereof and an SERS detection method.
Background
Since 1974 Fleischmann discovered a high-intensity Raman scattering phenomenon in the pyridine molecular structure on the surface of a rough silver electrode. In 2003, metal nanoparticles are attached to porous silicon and are verified to serve as SERS performance, in 2004, Haohao Lin synthesizes a silver nano-dendrite composite structure on the surface of the porous silicon by using a soaking method, and rhodamine R6G is used as a probe molecule to detect the SERS performance of the substrate. Until 2014, the preparation and performance of porous silicon composite metal nanostructures were again of interest.
AgNO by G H Jiang et al3And the PVP solution is slowly poured into the ethylene glycol which is refluxed at constant temperature (120 ℃) and magnetically stirred, the solution is brown after 10min, and a silver dendritic crystal structure with the length of 0.5-1 mu m and the width of 100-200 nm can grow after 1.5 h. The field of electrochemical corrosion with the frequency of 2450 and silicon microstructure preparation for Rong He and the like, and particularly relates to a novel porous silicon-silver nano dendrite particle and a preparation method thereof.
Microwave oven with MHz and 1000W power for removing radiation PVP and AgNO3And DMF to prepare dendritic silver nanostructures. X Zheng et al reduced Ag in microemulsions (containing surfactants) using vitamin C as a reducing agent+Thereby preparing the dendritic silver nanostructure. Jean Ming Xiao et al utilizes Raney Nickel and AgNO under ultrasonic conditions3Ag in solution+To prepare the silver dendritic structure.
At present, the traditional preparation methods of the silicon-metal structure comprise a photoinduction method, a polymer auxiliary method, a surfactant auxiliary method and the like, and the method for preparing the porous silicon-silver nano dendrite has complex processes and long time consumption, so that the SERS substrate is prepared. In addition, some researchers prepare porous silicon-metal structures by a thermal decomposition method, and thermal decomposition also needs to prepare a porous silicon sample firstly, soak porous silicon in a silver nitrate solution, take out the porous silicon immediately after the porous silicon is fully soaked in the solution, and then put the porous silicon sample into an oven to adjust the temperature to the thermal decomposition temperature of silver nitrate. The method has high requirement on environment, more steps and troublesome operation. The porous silicon-silver nano dendrite structure is troublesome in detection and has many limitations because the detected object needs to be dropped on a substrate for detection when the detected object is detected, and a preparation method of the porous silicon-silver nano dendrite particle is not reported in the research of a plurality of silicon-metal structures.
Disclosure of Invention
Aiming at the technical problems, the invention provides a porous silicon-silver nano dendrite particle and a preparation method thereof and an SERS detection method, the particle can be used as an SERS substrate for Raman detection, the preparation of the porous silicon-silver nano dendrite particle mainly comprises the steps of selecting a silicon wafer, cleaning the silicon wafer, preparing electrolytic corrosion liquid, electrifying for corrosion, preparing electrolytic separation liquid, electrifying for separation and ultrasonically shattering, firstly, the silicon wafer is ultrasonically cleaned by acetone, alcohol and deionized water respectively, so as to remove oil stains and impurities on the porous silicon; preparing electrolyte from hydrofluoric acid (HF), Dimethylformamide (DMF) and silver nitrate solution according to a certain proportion; then, carrying out electrochemical anodic corrosion on the silicon wafer; then adding hydrofluoric acid (HF) and ethanol (C)2H6O) preparing electrolyte according to a certain proportion to replace the original solution for electrochemical separation; finally, the sample is washed by deionized water and is placed into a container for ultrasonic vibration crushing. The method realizes the preparation of the porous silicon-silver nano dendrite particles for the first time, is convenient to operate, has simple steps, has low requirements on experimental environment, is short in time, and is suitable for rapidly preparing substrate particles for SERS performance biological detection in a large scale. The invention provides a stepwise synthesis preparation method, which is characterized in that a porous silicon-silver nano dendritic crystal particle structure is made into a particle state for the first time, and the flexible detection of a detected substance can be realized.
The technical scheme of the invention is as follows: a preparation method of porous silicon-silver nano dendrite particles comprises the following steps:
step S1, selecting a material: selecting a P-type silicon wafer, and cutting the silicon wafer into a plurality of small silicon wafers;
step S2, cleaning the sample: putting the silicon slice cut in the step S1 into an ultrasonic cleaning machine, and cleaning the silicon slice by using deionized water, alcohol and acetone in sequence to remove surface impurities and oil stains;
step S3, solution preparation: preparing an electrochemical corrosion solution, wherein the corrosion solution comprises 40 wt% of HF, DMF and a silver nitrate solution, and the 40 wt% of HF, DMF and the silver nitrate solution are mixed and prepared according to the proportion of 16:9: 8;
step S4, electrochemical corrosion: setting corrosion parameters, putting the silicon wafer cleaned in the step S2 into an anodic oxidation device containing the electrochemical corrosion solution in the step S3, and carrying out electrochemical anodic corrosion to form porous silicon-silver nano dendrites on the silicon wafer;
step S5, solution preparation: preparing an electrochemical corrosion solution, wherein the corrosion solution comprises ethanol and 40 wt% of HF solution, and the ethanol and the 40 wt% of HF solution are mixed and prepared according to the proportion of 14: 1;
step S6, electrochemical separation: setting corrosion parameters, putting the silicon wafer corroded in the step S4 into an anodic oxidation device containing the electrochemical corrosion liquid in the step S5, and performing electrochemical separation on the porous silicon-silver nano dendrites;
step S7, shattering the separated sample: and step S6, after the electrochemical separation is finished, taking out the silicon wafer, cleaning the corrosion area by deionized water, then putting the silicon wafer into a container containing ethanol solution, finally putting the silicon wafer into an ultrasonic instrument for ultrasonic shattering treatment, standing, taking out the silicon wafer, and leaving the porous silicon-silver nano dendrite particle solution.
In the above embodiment, in step S3, the electrochemical etching solution is prepared using a measuring cylinder on a table having a fume hood.
In the foregoing solution, the corrosion parameters in step S4 are: application of 40mA/cm2The etching time is 5 min.
In the above embodiment, in step S5, the electrochemical etching solution is prepared using a measuring cylinder on a table having a fume hood.
In the foregoing solution, the corrosion parameters in step S6 are: application of 22mA/cm2The etching time is 3 min.
A porous silicon-silver nano dendrite particle prepared according to the preparation method of the porous silicon-silver nano dendrite particle.
A SERS detection method based on porous silicon-silver nano dendrite particles comprises the following steps: use of the porous silicon-silver nano dendrite particle of claim 6 for SERS detection.
In the above scheme, the SERS detection method based on porous silicon-silver nano dendrite particles includes the following steps: and adding the measured substance into the solution containing the porous silicon-silver nano dendrite particles, soaking for 2-3 h, pouring the solution into a centrifuge tube, centrifuging for 10min at the rotating speed of 6000r/min, and performing SERS detection on the soaked porous silicon-silver nano dendrite particles with the measured substance.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a step-by-step synthesis method, which is used for preparing porous silicon-silver nano dendritic crystal particles. When the Raman detection is carried out, the traditional detection method is to drop the detected solution onto a substrate for detection, and the porous silicon-silver nano dendritic crystal particles can realize the detection of the solution, and can also drop the solution containing the particles onto the detected solid, and carry out the Raman detection after centrifugal drying or natural drying. Because the signal intensity of the substance to be detected is not very high, the particles increase the signal intensity of the substance to be detected, the Raman peak value is higher, the detection limit is higher, the traditional detection method is changed, and the flexibility and the diversity are higher when the substance is detected. The method can realize the preparation of the porous silicon-silver nano dendrite substrate under short corrosion time, and the prepared substrate has high SERS performance. The electrolyte used by the method is easy to purchase, easy to prepare, simple to operate and easy for large-scale production. The anodic oxidation device used in the method has the advantages of simple structure, easy operation, long-term use of the device and low cost.
Drawings
FIG. 1 is a 1000 SEM image of porous silicon-silver nano-dendrite particles prepared by the present invention;
FIG. 2 is a 4000-fold SEM image of porous silicon-silver nano-dendrite particles prepared by the present invention;
FIG. 3 is a 10000 times SEM image of porous silicon-silver nano-dendrite particles prepared by the present invention;
FIG. 4 is a 10000 times SEM image of porous silicon-silver nano-dendrite particles prepared by the present invention;
FIG. 5 is a Raman spectrum of the porous silicon-silver nano dendrite particles prepared by the method for detecting rhodamine.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
A preparation method of porous silicon-silver nano dendrite particles comprises the following steps:
step S1, selecting a material: selecting a P-type silicon wafer, and cutting the silicon wafer into square silicon wafers;
step S2, cleaning the sample: putting the square silicon slice cut in the step S1 into an ultrasonic cleaning machine, sequentially cleaning the silicon slice with deionized water, alcohol and acetone to remove surface impurities and oil stains, drying with a nitrogen gun, and sealing for storage for later use;
step S3, solution preparation: preparing an electrochemical corrosion solution on an operation table with a fume hood by using a measuring cylinder, wherein the corrosion solution comprises 40 wt% of HF, DMF and a silver nitrate solution, and the 40 wt% of HF, DMF and the silver nitrate solution are mixed and prepared according to the proportion of 16:9: 8;
step S4, electrochemical corrosion: setting corrosion parameters, putting the square silicon wafer cleaned in the step S2 into an anodic oxidation device containing the electrochemical corrosion solution in the step S3, and carrying out electrochemical anodic corrosion to form porous silicon-silver nano dendrites on the square silicon wafer;
step S5, solution preparation: preparing electrochemical corrosion solution on an operation table with a fume hood by using a measuring cylinder, wherein the corrosion solution comprises ethanol (C)2H6O) and 40 wt% HF solution, ethanol (C)2H6O) and 40 wt% HF solution are mixed according to the proportion of 14: 1;
step S6, electrochemical separation: setting corrosion parameters, putting the square silicon wafer corroded in the step S4 into an anodic oxidation device containing the electrochemical corrosion liquid in the step S5, and performing electrochemical separation on the porous silicon-silver nano dendrites;
step S7, shattering the separated sample: after the electrochemical separation in step S6 is completed, the square silicon wafer is taken out and the etched area is cleaned with deionized water, and then the square silicon wafer is placed in a container containing ethanol (C)2H6O) solution, and finally putting the solution into an ultrasonic instrument for ultrasonic shattering treatment. Standing for 24h, taking out the silicon wafer by using a clamp, and leaving the porous silicon-silver nano dendrite particle solution for sealing and storing for subsequent detection.
In step S3, an electrochemical etching solution is prepared using a measuring cylinder on a table having a fume hood.
The corrosion parameters in step S4 are: application of 40mA/cm2The etching time is 5 min.
In step S5, an electrochemical etching solution is prepared using a measuring cylinder on a table having a fume hood.
The corrosion parameters in step S6 are: application of 22mA/cm2The etching time is 3 min.
A porous silicon-silver nano dendrite particle prepared according to the preparation method of the porous silicon-silver nano dendrite particle.
A SERS detection method based on porous silicon-silver nano dendrite particles comprises the following steps: the porous silicon-silver nano dendrite particle is used for SERS detection, and comprises the following steps: and adding the measured substance into the solution containing the porous silicon-silver nano dendrite particles, soaking for 2-3 h, pouring the solution into a centrifuge tube, centrifuging for 10min at the rotating speed of 6000r/min, and performing SERS detection on the soaked porous silicon-silver nano dendrite particles with the measured substance.
According to the present embodiment, preferably, the step S1 selects the material: the silicon wafer is [100 ]]The resistivity of the crystal orientation P-type monocrystalline silicon is 10-20 omega cm2The thickness was 525 μm, and the silicon wafer was cut into a square silicon wafer of 1.5cm by a diamond cutter.
According to this embodiment, preferably, the step S2 washes the sample: and sequentially putting the cut square silicon wafer into a beaker filled with deionized water, alcohol and acetone for ultrasonic cleaning for 10 min.
According to this embodiment, preferably, the step S3 is to prepare: preparing electrochemical corrosion solution on an operation table with a fume hood, wherein the corrosion solution is prepared from 40 wt% of HF, DMF and AgNO3The solution was prepared at a ratio of 16:9:8, and 16ml HF, 9ml DMF and 8ml AgNO were taken out using a pipette3Putting the solution into a plastic measuring cylinder to prepare electrochemical corrosion solution, wherein the concentration of silver nitrate solution is 0.025M.
According to this embodiment, preferably, the step S4 is electrochemical etching: setting corrosion parameters, putting the square silicon wafer in the step S2 into an anodic oxidation device filled with electrolyte, and carrying out electrochemical anodic corrosion with the corrosion current of 40mA/cm2And the time is 5 min.
According to this embodiment, preferably, the step S5 — solution preparation: preparing electrochemical corrosion liquid on an operation table with a fume hood, wherein the corrosion liquid is composed of C2H6The O and HF solutions were mixed at a ratio of 14:1, and 14ml of C was taken out using a pipette2H6And putting the O and 1ml of HF solution into a plastic measuring cylinder to prepare the electrochemical corrosion solution.
According to this embodiment, preferably, the step S6 — electrochemical separation: setting corrosion parameters, putting the square silicon wafer in the step S4 into an anodic oxidation device containing the electrolyte in the step S5, and carrying out electrochemical anodic corrosion with the corrosion current of 22mA/cm2And the time is 3 min.
According to this embodiment, preferably, the step S7 — shattering the separated sample: after the electrochemical separation is finished, taking out the square silicon wafer, cleaning the corroded area by deionized water, and then putting the square silicon wafer into a container containing ethanol (C)2H6O) solution, finally placing the solution into an ultrasonic instrument for ultrasonic shattering for 10min, standing for 24h, taking out the silicon wafer by a clamp, leaving the porous silicon-silver nano dendrite particle solution, and sealing and storing for subsequent detection.
According to this embodiment, it is preferable that the porous silicon-silver nano dendrite particle solution prepared by the above experimental procedure is configured to contain R6G and porous silicon-A mixed solution of silver nano-dendrite particles having a concentration of R6G of 10-3M, soaking for 3 hours, pouring into a centrifuge tube for centrifugation, wherein the centrifugation speed is 6000R/min, the centrifugation time is 10min, then pouring out the supernatant to obtain centrifuged particles, and finally performing SERS detection of R6G.
And (4) analyzing results:
the appearance of the experimental sample is tested. Fig. 1 shows the size of the porous silicon-silver nano-dendrite particles under this preparation condition, and it can be seen that the size of the porous silicon-silver nano-dendrite particles is mostly less than 60 μm. FIG. 2 is a schematic view of the porous silicon-silver nano-dendrite particle structure showing the etched porous silicon substrate on the bottom, the grown silver dendrite on the top, and the grown silver particle in the middle of the connection. FIG. 3 is an SEM image of the structure of an upper porous silicon-silver nano dendrite particle, where a is a growing silver dendrite and b is a growing silver particle, and a substance to be detected can combine with the porous silicon-silver nano dendrite particles at a and b to increase the SERS signal for Raman detection. FIG. 4 is an SEM image of the structure of the underlying porous silicon-silver nano-dendrite particles, where the porous silicon-silver nano-dendrite particles are the silver particles grown where the silicon substrate joins the silver dendrites, and where the particles are the silicon substrate. FIG. 5 is a Raman spectrum of the porous silicon-silver nano dendrite structure on R6G SERS detection, wherein the concentration of R6G in the experiment is 10-3M, at 610cm-1,770cm-1,1361cm-11,1507cm-1And 1572cm-1And 1649cm-1The spectral characteristic peak and the peak value of R6G are clearly enhanced, the SERS intensity is greatly improved, and the substrate of the porous silicon-silver dendrite particle has excellent SERS performance. The porous silicon-silver nano dendrite particles can realize the detection of the solution, and can also drop the particle solution onto a detected solid, and carry out Raman detection after the particle solution is naturally dried, so that the traditional detection method is changed, and the detection method has more flexibility when detecting substances.
It should be understood that although the present description has been described in terms of various embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and those skilled in the art will recognize that the embodiments described herein may be combined as suitable to form other embodiments, as will be appreciated by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.

Claims (8)

1. A preparation method of porous silicon-silver nano dendrite particles is characterized by comprising the following steps:
step S1, selecting a material: selecting a P-type silicon wafer, and cutting the silicon wafer into a plurality of small silicon wafers;
step S2, cleaning the sample: putting the silicon slice cut in the step S1 into an ultrasonic cleaning machine, and cleaning the silicon slice by using deionized water, alcohol and acetone in sequence to remove surface impurities and oil stains;
step S3, solution preparation: preparing an electrochemical corrosion solution, wherein the corrosion solution comprises 40 wt% of HF, DMF and a silver nitrate solution, and the 40 wt% of HF, DMF and the silver nitrate solution are mixed and prepared according to the proportion of 16:9: 8;
step S4, electrochemical corrosion: setting corrosion parameters, putting the silicon wafer cleaned in the step S2 into an anodic oxidation device containing the electrochemical corrosion solution in the step S3, and carrying out electrochemical anodic corrosion to form porous silicon-silver nano dendrites on the silicon wafer;
step S5, solution preparation: preparing an electrochemical corrosion solution, wherein the corrosion solution comprises ethanol and 40 wt% of HF solution, and the ethanol and the 40 wt% of HF solution are mixed and prepared according to the proportion of 14: 1;
step S6, electrochemical separation: setting corrosion parameters, putting the silicon wafer corroded in the step S4 into an anodic oxidation device containing the electrochemical corrosion liquid in the step S5, and performing electrochemical separation on the porous silicon-silver nano dendrites;
step S7, shattering the separated sample: and step S6, after the electrochemical separation is finished, taking out the silicon wafer, cleaning the corrosion area by deionized water, then putting the silicon wafer into a container containing ethanol solution, finally putting the silicon wafer into an ultrasonic instrument for ultrasonic shattering treatment, standing, taking out the silicon wafer, and leaving the porous silicon-silver nano dendrite particle solution.
2. The method for preparing porous silicon-silver nano dendrite particles of claim 1 wherein step S3 is to use a measuring cylinder to prepare electrochemical etching solution on a bench with a fume hood.
3. The method for preparing porous silicon-silver nano dendrite particles according to claim 1 wherein the etching parameters in step S4 are: application of 40mA/cm2The etching time is 5 min.
4. The method for preparing porous silicon-silver nano dendrite particles of claim 1 wherein step S5 is to use a measuring cylinder to prepare electrochemical etching solution on a bench with a fume hood.
5. The method for preparing porous silicon-silver nano dendrite particles according to claim 1 wherein the etching parameters in step S6 are: application of 22mA/cm2The etching time is 3 min.
6. A porous silicon-silver nano dendrite particle prepared by the method of preparing a porous silicon-silver nano dendrite particle according to any one of claims 1 to 5.
7. A SERS detection method based on porous silicon-silver nano dendrite particles is characterized by comprising the following steps: use of the porous silicon-silver nano dendrite particle of claim 6 for SERS detection.
8. The method for SERS detection based on porous silicon-silver nano-dendrite particles according to claim 7, comprising the steps of: and adding the measured substance into the solution containing the porous silicon-silver nano dendrite particles, soaking for 2-3 h, pouring the solution into a centrifuge tube, centrifuging for 10min at the rotating speed of 6000r/min, and performing SERS detection on the soaked porous silicon-silver nano dendrite particles with the measured substance.
CN202110780137.3A 2021-07-09 2021-07-09 Porous silicon-silver nano dendrite particle, preparation method thereof and SERS detection method Pending CN113638035A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101778796A (en) * 2007-04-27 2010-07-14 得克萨斯大学体系董事会 porous particles and methods of making thereof
CN103890915A (en) * 2011-08-19 2014-06-25 威廉马歇莱思大学 Anode battery materials and methods of making the same
CN105264654A (en) * 2013-01-07 2016-01-20 威廉马歇莱思大学 Combined electrochemical and chemical etching processes for generation of porous silicon particulates
CN105290394A (en) * 2015-11-03 2016-02-03 宁波大学 Silver-mesoporous silica-silver sandwich core shell nanometer material and preparation and application thereof
CN105562714A (en) * 2016-02-03 2016-05-11 宁波大学 Nanometer material for SERS (Surface-Enhanced Raman Scattering) detection and preparing method of nanometer material
CN110331427A (en) * 2019-06-10 2019-10-15 江苏大学 A kind of porous silicon-silver nanoparticle pine-tree structure and preparation method thereof
CN111965158A (en) * 2020-07-13 2020-11-20 江苏大学 Single-step rapid preparation method of porous silicon-gold dendritic crystal composite structure

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101778796A (en) * 2007-04-27 2010-07-14 得克萨斯大学体系董事会 porous particles and methods of making thereof
CN103890915A (en) * 2011-08-19 2014-06-25 威廉马歇莱思大学 Anode battery materials and methods of making the same
CN105264654A (en) * 2013-01-07 2016-01-20 威廉马歇莱思大学 Combined electrochemical and chemical etching processes for generation of porous silicon particulates
CN105290394A (en) * 2015-11-03 2016-02-03 宁波大学 Silver-mesoporous silica-silver sandwich core shell nanometer material and preparation and application thereof
CN105562714A (en) * 2016-02-03 2016-05-11 宁波大学 Nanometer material for SERS (Surface-Enhanced Raman Scattering) detection and preparing method of nanometer material
CN110331427A (en) * 2019-06-10 2019-10-15 江苏大学 A kind of porous silicon-silver nanoparticle pine-tree structure and preparation method thereof
CN111965158A (en) * 2020-07-13 2020-11-20 江苏大学 Single-step rapid preparation method of porous silicon-gold dendritic crystal composite structure

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