CN112609164A - Method for preparing porous metal nanoparticles by laser - Google Patents
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Abstract
The invention provides a method for preparing porous metal nano particles by laser, which comprises the following steps: s1: taking a transparent glass sheet for plasma cleaning; s2: carrying out magnetron sputtering on the metal A nanometer film and the metal B nanometer film on the surface of the glass sheet in sequence; s3: adding an acid solution into the receiving groove, and flatly placing the surface of the glass sheet plated with the metal A nano film and the metal B nano film on the liquid level of the receiving groove; s4: the nano-film of the metal A and the nano-film of the metal B are focused by nanosecond laser to perform ablation, so that the alloy AB nano-particles are formed, and simultaneously, the porous metal B nano-particles are directly obtained after the metal A is etched under the action of an acid solution. The invention provides a method for preparing porous metal nano particles by gas-liquid interface laser induction, which has the advantages of adjustable porosity, adjustable types of porous nano particles, simple method and capability of being used for rapid large-scale preparation.
Description
Technical Field
The invention relates to the technical field of preparation of nano functional structures/materials, in particular to a method for preparing porous metal nanoparticles by laser.
Background
The porous metal nanoparticles are highly valued for their excellent properties and wide applications, and have characteristics of large surface area, low density, cavities and surface pores, and controllable morphology and composition. At present, common methods for preparing porous metal nanoparticles include an electrochemical displacement reaction method, a kirkendall effect, an etching method, and the like. As disclosed in chinese patent publication No.: CN 106811750 a, patent publication date: 2017.06.09, providing a magnesium-based alloy strip, wherein the main structure of the magnesium-based alloy strip is an amorphous phase, the stoichiometric atomic formula of the magnesium-based alloy strip is MgaXbMcRd, R is a rare earth element or a mixture of the rare earth element and other active elements, the MgaXbMcRd contains at least one of Cu and Ni, wherein a is more than or equal to 40% and less than or equal to 80%, b is more than or equal to 5% and less than or equal to 30%, c is more than or equal to 5% and less than or equal to 30%, d is more than or equal to 1% and less than or equal to 30%, and a + b + c + d is 100%; secondly, performing a first dealloying reaction on the magnesium-based alloy strip and a first acid solution, and reacting Mg and R type atoms in the magnesium-based alloy strip with hydrogen ions in the first acid solution to form a nano-porous metal strip, wherein the nano-porous metal strip contains X atoms and M atoms; thirdly, adding the nano-porous metal strip into a second acid solution, and simultaneously carrying out a second alloy removing reaction by ultrasonic waves, so that M atoms in the nano-porous metal strip react with hydrogen ions in the second acid solution to form nano-porous metal particles.
Although the chemical method can realize high-yield preparation, other chemical products are often required to be separated after the synthesis is finished, and the problems of complicated operation, impure products and the like exist. In the practical application process, a preparation method which can realize large-scale production of the nano particles and is cleaner and simpler is needed to meet various requirements of the nano particles.
As the technology of laser in micro-nano fine processing becomes more and more mature, people also apply laser processing to the preparation of nano-particles. In the field of Laser micro-nano fine processing, the most prominent advantage of the Laser ablation in liquid, LAL (Laser ablation in liquid) technology is the purity of the product, no other impurities generated by chemical reaction are generated, and meanwhile, the yield of nanoparticles is improved, and the applicable material range is greatly improved. However, the process is affected by various factors such as laser, target material, liquid and the like, and physical properties such as size, shape, polymerization degree and the like of the prepared nanoparticles cannot be controlled more accurately, so that requirements on the nanoparticles under different conditions are met, and the process is a challenge for preparing the nanoparticles by LAL at present.
Laser-induced forward transfer (LIFT) technology mainly uses Laser to penetrate through a transparent source substrate to act on a thin film on the other surface of a substrate, so that a thin film material is peeled off and deposited on another target substrate below to realize material substance transfer. Compared with LAL, LIFT eliminates uncertain influence caused by laser passing through a liquid environment, controllability is higher, but nanoparticles prepared by LIFT cannot reach smaller size without the assistance of liquid.
Disclosure of Invention
In order to overcome the problems of complex operation and large prepared nano particles in the prior art, the invention provides a method for preparing porous metal nano particles by laser, which has a simple production method and can be used for rapid large-scale preparation, and the prepared nano particles reach smaller sizes.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for preparing porous metal nanoparticles by laser comprises the following steps:
s1: taking a transparent glass sheet 2 for plasma cleaning;
s2: carrying out magnetron sputtering on the surface of the glass sheet 2 to form a metal A nanometer film 3 and a metal B nanometer film 4 in sequence;
s3: adding an acid solution into the receiving groove 7, and flatly placing the surface of the glass sheet 2 plated with the metal A nano film 3 and the metal B nano film 4 on the liquid surface of the receiving groove 7;
s4: the nano-film 3 of the metal A and the nano-film 4 of the metal B are focused by nanosecond laser 1 to be ablated, so that alloy AB nano-particles are formed, and simultaneously, the nano-particles of the porous metal B are directly obtained after the metal A is etched under the action of an acid solution.
Preferably, after step S4, a surface dispersant may be added to improve the dispersibility of the porous metal B nanoparticles.
Preferably, the glass sheet is made of quartz glass.
Preferably, the thicknesses of the metal A nano film 3 and the metal B nano film 4 are 50-500 nm, wherein the metal A nano film is used as a final sacrificial template, and the thickness ratio of the metal A nano film to the metal B nano film is 1: n, wherein N is greater than 0.
Preferably, in step S2, the metal a nano-film is magnetron sputtered on the surface of the glass sheet, and then the metal B nano-film is magnetron sputtered on the surface of the glass sheet.
Preferably, in step S4, the wavelength of the nanosecond laser is 1064nm, the scanning speed of the nanosecond laser is 200-2000 mm/S, the pulse frequency of the nanosecond laser is 10-50 kHz, the pulse power of the nanosecond laser is 6-21W, and the space between the filling lines is 0.01-0.05 mm.
Preferably, the concentration of the acid solution is 0.1-5.0 mol/L.
Further, the surface dispersant includes, but is not limited to, any one of polyvinylpyrrolidone and methoxy-polyethylene glycol-mercapto group having acid resistance.
Preferably, the receiving groove is made of transparent high polymer or high polymer material which is not sensitive to laser.
Furthermore, the receiving groove is prepared by adopting polydimethylsiloxane.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
according to the method for preparing the porous metal nano-particles by using the laser, the prepared porous metal nano-particles have the following advantages: the porosity is adjustable, the metal proportion in the alloy nano-particles can be flexibly controlled by controlling the thickness proportion of the magnetron sputtering metal nano-film A, B, and then porous metal nano-particles with different porosities are obtained; secondly, the types of the porous metal nano particles are adjustable; thirdly, the method is simple and can be used for rapid large-scale preparation. Moreover, the nano-porous metal particles can reach smaller size by ablation through nanosecond laser; the porous metal nanoparticles have high specific surface area and strong hot spot effect, and can be widely applied to the biological fields of surface enhanced Raman signals, drug transportation and the like.
Drawings
Fig. 1 is a preparation flow chart of the method for laser preparing porous metal nanoparticles in example 1.
Fig. 2 is a schematic diagram of a method for laser-preparing porous metal nanoparticles in example.
Fig. 3 is a graph of the ultraviolet-visible light spectrum of the gold-silver nano alloy particles with different proportions in example 2.
FIG. 4 is a graph of the UV-Vis spectra of the Au/Ag nanoparticles of example 2 with different mixing ratios.
In the figure, 1-nanosecond laser, 2-glass sheet, 3-metal A nano film, 4-metal B nano film, 5-porous metal B nano particle, 6-acid solution and 7-receiving groove.
Detailed Description
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 only a part of the embodiments of the present invention, and are used for illustration only, and should not be construed as limiting the patent. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical solution of the present invention is further described below with reference to the accompanying drawings and examples.
Example 1
As shown in fig. 1, a method for preparing porous metal nanoparticles by laser comprises the following steps:
s1: taking a transparent glass sheet 2 for plasma cleaning; the glass sheet described in this example is preferably quartz glass.
S2: carrying out magnetron sputtering on the surface of the glass sheet 2 to form a metal A nanometer film 3 and a metal B nanometer film 4 in sequence; the thicknesses of the metal A nano film 3 and the metal B nano film 4 are 50-500 nm, wherein the metal A nano film 3 is used as a final sacrificial template, and the thickness ratio of the metal A nano film 3 to the metal B nano film 4 is 1: n, wherein N is greater than 0. The surface of the glass sheet 2 is firstly coated with the metal A nanometer film 3 by magnetron sputtering and then coated with the metal B nanometer film 4 by magnetron sputtering.
S3: adding an acid solution into the receiving groove 7, and flatly placing the surface of the glass sheet 2 plated with the metal A nano film 3 and the metal B nano film 4 on the liquid surface of the receiving groove 7; the acid solution adopted by the embodiment can corrode the metal A and is difficult to corrode the metal B, and the concentration of the acid solution is 0.1-5.0 mol/L. The receiving groove 7 is made of transparent high polymer or high polymer material insensitive to laser. The receiving groove 7 is made of polydimethylsiloxane.
S4: the nano-film 3 of the metal A and the nano-film 4 of the metal B are focused by nanosecond laser 1 to be ablated, alloy AB nano-particles are formed, and simultaneously, the nano-particles 5 of the porous metal B are directly obtained after the metal A is etched under the action of an acid solution. In a specific embodiment, the wavelength of the nanosecond laser 1 is 1064nm, the scanning speed of the nanosecond laser 1 is 200-2000 mm/s, the pulse frequency of the nanosecond laser 1 is 10-50 kHz, the pulse power of the nanosecond laser 1 is 6-21W, and the line spacing is 0.01-0.05 mm.
In a specific embodiment, after step S4, a surface dispersant may be added to improve the dispersibility of the porous metal B nanoparticles 5. The surface dispersant includes but is not limited to any one of polyvinylpyrrolidone and methoxy-polyethylene glycol-mercapto group with acid resistance.
Example 2
Based on the method described in example 1, this example is described in detail with reference to specific applications,
s1: mixing 5 pieces of 75 × 25mm × 1.3mm3The quartz glass is treated for 5min in a plasma cleaning machine with the frequency of 13.56MHz, and the glass sheets are respectively numbered from the first step to the fifth step:
s2: then, a magnetron sputtering film plating machine is used for respectively carrying out magnetron sputtering on the silver (Ag) nano film and the gold (Au) nano film on the glass sheet in sequence. The overall thickness of the metal nano film from the glass sheet I to the glass sheet II is 200 nm; wherein the thickness of the Ag nano film is respectively 200nm, 150nm, 100nm, 50nm and 0nm in sequence, and the thickness of the Au nano film is respectively 0nm, 50nm, 100nm, 150nm and 200nm in sequence.
S3: adopting a receiving tank prepared by Polydimethylsiloxane (PDMS), adding 800 mu L of deionized water solution into the receiving tank, spreading one surface of a glass sheet of the magnetron sputtering metal nano-film on the deionized water solution,
s4: the nanosecond laser is focused on the interface of the metal nanometer film and the deionized water solution, and the nanosecond laser parameters are as follows: the nanosecond laser has a wavelength of 1064nm, a maximum pulse power of 30W and a pulse energy of 1mJ, and in this example, a scanning speed of 1000mm/s, a pulse frequency of 30kHz, a pulse power of 35% of the maximum pulse power, a scanning pattern of 8 × 8mm2 squares, and a space between the filling lines of 0.03mm are set. After the laser scanning is completed once, the glass sheet is removed, and the gold/silver nano (alloy) particle solution dispersed in the receiving tank is collected by using a liquid-transferring gun.
Referring to the schematic diagram of the laser preparation method of porous metal nanoparticles in fig. 2, the laser beam is focused on the interface between the metal nano-film and the liquid through the quartz glass plate, and the resulting gold/silver nano (alloy) particle product is dispersed in the receiving liquid below.
Referring to the ultraviolet-visible light spectrograms of gold-silver nano alloy particles with different proportions in FIG. 3, the Nano Particles (NPs) obtained by laser ablation of a glass sheet containing a gold-silver nano film are respectively Ag and Ag150Au50、Ag100Au100、 Ag50Au150And the Local Surface Plasmon Resonance (LSPR) absorption peaks of the Au are 407nm, 426nm, 460nm, 496nm and 523nm in sequence. As can be seen from FIG. 3, each NPs solution has only one LSPR absorption peak, which indicates that the prepared NPs are alloysAnd the absorption peak gradually red-shifted as the Au ratio increased.
Referring to the ultraviolet-visible spectrum of gold/silver nanoparticles with different mixing ratios in fig. 4, it is further demonstrated that the prepared NPs are alloys. Firstly, preparing Ag NPs and Au NPs respectively, and mixing the Ag NPs and the Au NPs in a ratio of 1:0, 3:1, 1:3 and 0:1 in sequence. As is clear from FIG. 4, when Ag NPs and Au NPs were mixed, LSPR absorption peaks were observed at 407nm and 523 nm. It is further demonstrated that the NPs prepared in fig. 3 are alloys.
And in addition, the deionized water in the receiving tank is replaced by 1mol/L nitric acid solution which can etch the Ag element but is inert to Au, the operation steps are the same as the steps S3 and S4, the Ag/Au nano film is ablated by nanosecond laser, after AgAu alloy nano particles are formed, the Ag element is etched by the nitric acid solution instantly, and the porous Au NPs solution is obtained in one step directly. A1.5 mL centrifuge tube is used for storing the porous Au NPs solution, 200 mu L of 1mM methoxy-polyethylene glycol-mercapto (mPEG-SH) is added, and the reaction is carried out for 30min in a vortex oscillator with the rotating speed of 5000rpm, so that the stability and the dispersibility of the porous Au NPs are improved. And porous AuNPs with different porosities can be prepared by regulating the thickness ratio of the initial Ag/Au nano-film.
Example 3
The preparation of the porous platinum (Pt) nanoparticles can also be described in detail below by preparing the desired porous metal nanoparticles by matching different metals.
1 piece of 75X 25mm X1.3 mm3The quartz glass is treated for 5min in a plasma cleaning machine with the frequency of 13.56MHz, and then an Ag nano film with the thickness of 150nm and a 50nmPt nano film are respectively sputtered on a glass sheet by a magnetron sputtering film plating machine in a magnetron way.
Referring to fig. 2, 800 μ L of a 1mol/L nitric acid solution, which can etch Ag element but is inert to Au, is added into the PDMS receiving groove. One surface of a glass sheet for magnetron sputtering of the Pt/Ag nano film is flatly laid on a liquid surface, laser is focused on an interface of the gold Pt/Ag nano film and the liquid, and nanosecond laser parameters are as follows: the laser wavelength is 1064nm, the maximum pulse power is 30W, the pulse energy is 1mJ, the scanning speed is 1000mm/s, the frequency is 30kHz, the laser power output is 35 percent in the experiment, the scanning pattern is a square of 8 multiplied by 8mm2, and the space between the filling lines is 0.03 mm. After laser scanning is finished once, AgPt alloy nanoparticles are formed, the Ag element is etched by nitric acid instantly, and porous Pt NPs solution is directly obtained in one step. A1.5 mL centrifuge tube is used for storing the porous Pt NPs solution, 200 mu L of 1mM methoxy-polyethylene glycol-mercapto (mPEG-SH) is added, and the reaction is carried out for 30min in a vortex oscillator with the rotating speed of 5000rpm, so that the stability and the dispersibility of the porous Pt NPs are improved. And porous Pt NPs with different porosities can be prepared by regulating the thickness ratio of the initial Ag/Pt nano film. The glass slide was removed and the dispersed porous Pt NPs solution in the receiving cell was collected with a pipette.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A method for preparing porous metal nano-particles by laser is characterized by comprising the following steps: the method comprises the following steps:
s1: taking a transparent glass sheet for plasma cleaning;
s2: carrying out magnetron sputtering on the metal A nanometer film and the metal B nanometer film on the surface of the glass sheet in sequence;
s3: adding an acid solution into the receiving groove, and flatly placing the surface of the glass sheet plated with the metal A nano film and the metal B nano film on the liquid level of the receiving groove;
s4: the nano-film of the metal A and the nano-film of the metal B are focused by nanosecond laser to perform ablation, so that the alloy AB nano-particles are formed, and simultaneously, the porous metal B nano-particles are directly obtained after the metal A is etched under the action of an acid solution.
2. The method for laser preparing porous metal nanoparticles according to claim 1, wherein: after step S4, a surface dispersant may be added to improve the dispersibility of the porous metal B nanoparticles.
3. The method for laser preparing porous metal nanoparticles according to claim 1, wherein: the glass sheet is made of quartz glass.
4. The method for laser preparing porous metal nanoparticles according to claim 1, wherein: the thickness of the metal A nano film and the thickness of the metal B nano film are 50-500 nm, wherein the metal A nano film is used as a final sacrificial template, and the thickness ratio of the metal A nano film to the metal B nano film is 1: n, wherein N is greater than 0.
5. The method for laser preparing porous metal nanoparticles according to claim 1, wherein: in step S2, a metal a nano-film is first magnetron sputtered on the surface of the glass sheet, and then a metal B nano-film is magnetron sputtered on the surface of the glass sheet.
6. The method for laser preparing porous metal nanoparticles according to claim 1, wherein: and S4, wherein the wavelength of the nanosecond laser is 1064nm, the scanning speed of the nanosecond laser is 200-2000 mm/S, the pulse frequency of the nanosecond laser is 10-50 kHz, the pulse power of the nanosecond laser is 6-21W, and the line spacing is 0.01-0.05 mm.
7. The method for laser preparing porous metal nanoparticles according to claim 1, wherein: the concentration of the acid solution is 0.1-5.0 mol/L.
8. The method for laser preparing porous metal nanoparticles according to claim 2, wherein: the surface dispersant includes but is not limited to any one of polyvinylpyrrolidone and methoxy-polyethylene glycol-mercapto group with acid resistance.
9. The method for laser preparing porous metal nanoparticles according to claim 1, wherein: the receiving groove is made of transparent high polymer or high polymer material insensitive to laser.
10. The method for laser preparing porous metal nanoparticles according to claim 9, wherein: the receiving groove is prepared by adopting polydimethylsiloxane.
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| CN115283685A (en) * | 2022-08-18 | 2022-11-04 | 北京科技大学 | Method for preparing high-entropy alloy nanoparticles by laser |
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