CN110640149B - Method for preparing nano alloy particles by laser induction - Google Patents
Method for preparing nano alloy particles by laser induction Download PDFInfo
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- CN110640149B CN110640149B CN201910885828.2A CN201910885828A CN110640149B CN 110640149 B CN110640149 B CN 110640149B CN 201910885828 A CN201910885828 A CN 201910885828A CN 110640149 B CN110640149 B CN 110640149B
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Abstract
The invention provides a method for preparing nano alloy particles by laser induction, which comprises the following steps: step 1, adding at least two metal nano material solutions into a centrifugal tube, and adding a proper amount of volatile solvent to form a mixed solution; step 2, ultrasonically mixing the solution to uniformly mix all the metal nano materials; step 3, centrifugally concentrating the mixed solution after ultrasonic treatment to obtain nano slurry; step 4, spin-coating the nano-slurry on the substrate; step 5, carrying out vacuum heating drying on the substrate after the spin coating is finished, and forming a dry coating layer on the surface of the substrate; and 6, pressing the light-transmitting sheet on the surface of the substrate with the dry coating layer, and then scanning the metal nano material on the substrate by passing laser through the light-transmitting sheet to obtain the nano alloy particles, wherein the power of the laser is not lower than 220mW, and the diameter of a light spot is larger than 70 um. The method has the advantages of good repeatability, high production speed, high efficiency, short time consumption, simple operation and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of nano functional structures/materials, and particularly relates to a method for preparing nano alloy particles by laser induction.
Background
The nano alloy particles are widely concerned in the fields of catalysis, energy storage, biological imaging, plasma imaging and the like. The preparation method of the large-area nano alloy particles can effectively promote the development of science and technology.
The present researchers invented many methods for preparing nano alloy particles, such as wet synthesis, carbon thermal oscillation, and scanning probe block polymer lithography, but these methods all have certain drawbacks. For example, the wet synthesis and the scanning probe block polymer have slow photoetching speed and low efficiency; carbon thermal shock is fast and the prepared nano alloy particles can contain eight metals, but the equipment is very expensive, so the method is not suitable for large-scale mass production due to harsh operating conditions.
Disclosure of Invention
The present invention is made to solve the above problems, and an object of the present invention is to provide a method for laser-induced preparation of nano-alloy particles.
In order to achieve the purpose, the invention adopts the following scheme:
the invention provides a method for preparing nano alloy particles by laser induction, which is characterized by comprising the following steps of: step 1, adding at least two metal nano material solutions into a centrifugal tube, and adding a proper amount of volatile solvent to form a mixed solution; step 2, ultrasonically mixing the solution to uniformly mix all the metal nano materials; step 3, centrifugally concentrating the mixed solution after ultrasonic treatment to obtain nano slurry; step 4, spin-coating the nano-slurry on the substrate; step 5, carrying out vacuum heating drying on the substrate after the spin coating is finished, and forming a dry coating layer on the surface of the substrate; and 6, pressing the light-transmitting sheet on the surface of the substrate with the dry coating layer, and then scanning the metal nano material on the substrate by passing laser through the light-transmitting sheet to obtain the nano alloy particles, wherein the power of the laser is not lower than 220mW, and the diameter of a light spot is larger than 70 um.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the step 1, the adopted metal nano material is metal nano particles or metal nano wire material or a mixed material of the metal nano particles and the metal nano wire material, the diameter of the metal nano particles is 10-600 nm, the diameter of the metal nano wires is 10-800 nm, and the surfaces of the nano wires are not coated with a dispersing agent.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the step 1, the volatile solvent is any one or a mixture of several of alcohols, ketones, benzenes, chloroform and deionized water.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in step 1, the ratio of the volume of the mixed solution to the volume of the metal nanomaterial solution is greater than 1:1, more preferably 3: 1-15: 1.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the step 2, the ultrasonic time is 5min to 40 min; the ultrasonic power is more than 70W, and more preferably 80W-100W.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the step 3, the centrifugal rotating speed of the centrifugal concentration is 2000-15000 rad/min, the centrifugal time is 2-10 min, and the volume of the centrifuged nano slurry is 5-25% of the volume of the mixed solution.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in step 4, the spin coating speed is 100rad/min to 6000rad/min, and the spin coating time is 5s to 60 s.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in step 4, the substrate is a metal substrate with a smooth and flat polished surface, and the surface roughness grade should be less than 0.1.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the step 5, the temperature of vacuum heating and drying is 30-65 ℃ for 5-1800 s.
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the step 6, the adopted laser is nanosecond laser, picosecond laser or femtosecond laser, the scanning speed of the laser is 20-2000 mm/s, the diameter of a light spot is 70-200 um, the pulse frequency of the laser is 10-200 k, the pulse width is 50 fs-200 ns, the wavelength of the laser is 248-1064 nm, and the power of the laser is 220 mW-5000 mW.
Action and Effect of the invention
The method for preparing the nano alloy particles by laser induction comprises the steps of sequentially adding corresponding metal nano materials into a volatile solvent, obtaining uniformly mixed metal nano slurry by an ultrasonic and centrifugal method, spin-coating the metal nano slurry on a substrate, placing a light-transmitting sheet on the substrate after the solvent is completely volatilized, and scanning the metal nano mixed material through the light-transmitting sheet by adopting laser with the power of not less than 220mW and the spot diameter of more than 70 microns to obtain the nano alloy particles.
Drawings
FIG. 1 is a flowchart illustrating the operation of a method for preparing nano-alloy particles by laser induction according to an embodiment of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of silver nanoparticles used in one embodiment of the invention;
FIG. 3 is a scanning electron micrograph of copper nanowires employed in an embodiment of the present invention;
FIG. 4 is a scanning electron microscope image of silver-copper nano-alloy particles prepared in the first embodiment of the invention;
FIG. 5 is a diagram of an energy spectrum analysis (EDS) element of a single particle nano-alloy prepared in the first example of the present invention.
FIG. 6 is a scanning electron microscope image of silver nanowires employed in the second embodiment of the present invention;
FIG. 7 is a scanning electron microscope image of silver-copper nano-alloy particles prepared in example II of the present invention;
FIG. 8 is a diagram of energy spectrum analysis (EDS) elements of a single particle nano-alloy prepared in example two of the present invention.
The reference numbers in the figures above mean:
100-a suction pipe, 101-a centrifuge tube, 102-a first metal nano material solution, 103-a first metal nano material solution, 104-a mixed solution of two metal nano materials, 105-a volatile solvent, 106-a mixed solution of a metal nano material and a volatile solvent, 107-an ultrasonic cleaning machine, 108-deionized water, 109-a centrifuge, 110-a supernatant, 111-a metal nano slurry, 112-a substrate, 113-a laser device, 114-a laser, 115-a light-transmitting sheet, 116-a dried metal nano mixed material, and 117-nano alloy particles.
Detailed Description
The following describes in detail specific embodiments of the laser-induced preparation method of nano-alloy particles according to the present invention with reference to the accompanying drawings.
< example one >
As shown in fig. 1, the method for preparing nano alloy particles by laser induction provided in this embodiment specifically includes the following steps:
s1-1, transferring the solution 102 of the first metal nano material into a centrifuge tube 101 by using a pipette 100; in the first embodiment, the first metal nano-material is the silver nano-particles shown in fig. 2, the solvent is absolute ethyl alcohol (99.7 wt.%), the volume of the whole solution 102 is 900ul, the concentration is 0.1mg/ml, and the volume of the centrifuge tube 101 is 4 ml;
s1-2, transferring the second metal nano material solution 103 into a centrifugal tube 101 by using a pipette 100 to form a mixed solution 104 of the two metal nano materials; in the first embodiment, the second metal nano-material is the copper nanowire shown in fig. 3, the solvent is absolute ethyl alcohol (99.7 wt.%), the volume of the whole solution 103 is 300ul, and the concentration is 10 mg/m;
s1-3, adding the volatile solvent 105 into the centrifuge tube 101 by using a pipette 100 to form a mixed solution 106; in the first embodiment, a pipette 100 is used to add alcohol to the 4ml mark of the centrifuge tube 101;
s2, placing the centrifugal tube 101 in an ultrasonic cleaning machine 107 for ultrasonic treatment, wherein in the first embodiment, the ultrasonic power is set to be 100W, and the ultrasonic time is set to be 20 min;
s3-1, after the ultrasonic treatment is finished, taking out the centrifugal tube 101, and placing the centrifugal tube in a centrifugal machine 109 for centrifugation, wherein in the first embodiment, the centrifugation speed is 10000r/min, and the centrifugation time is 6 min;
s3-2, after the centrifugation is finished, removing the supernatant 110, and leaving the high-concentration metal nano slurry 111; in this example one, after centrifugation, 3.5ml of the supernatant was removed with a pipette;
s4, spin-coating the high-purity metal nano-slurry 111 on a substrate 112, wherein in the first embodiment, the rotation speed of a spin-coating machine is set to be 300rad/min, the rotation time is set to be 30s, and the substrate 112 is a metal aluminum sheet with a smooth surface and a roughness grade of less than 0.1;
s5, carrying out vacuum heating drying on the substrate 112, in the first embodiment, putting the substrate 112 into a vacuum drying oven, wherein the temperature of the drying oven is 50 ℃, the time is 5min, taking out the substrate 112 after the solvent is completely volatilized, and forming a dried metal nano mixed material 116 on the surface of the substrate 112;
s6-1, placing a light-transmitting sheet 115 on the substrate 112, passing the laser 114 through the light-transmitting sheet 115, and scanning the dried metal nano-hybrid material 116; in the first embodiment, a transparent glass plate is used as the light-transmitting plate 115, and is placed on the substrate 112 to press the metal nano-hybrid material 116; the adopted laser is nanosecond laser, the wavelength of the laser is 1064nm, the power of the laser is 250mW, the scanning speed is 500mm/s, the diameter of a light spot is 78um, the pulse frequency of the laser is 20k, and the pulse width is 115 ns;
and S6-2, obtaining the nano alloy particles 117 after the laser 114 scanning is finished.
And (3) performance characterization:
as shown in fig. 4, as can be seen from the scanning electron microscope image, the diameter of the nano-alloy particles prepared in the first embodiment is 50nm to 1000nm, the shape is regular, and no obvious cavity is formed on the surface. As shown in fig. 5, it was confirmed by energy spectrum analysis that the nano-alloy particles prepared in the first example contained two metal elements of silver and copper.
< example two >
As shown in fig. 1, the method for preparing nano alloy particles by laser induction provided in the second embodiment specifically includes the following steps:
s1-1, transferring the solution 102 of the first metal nano material into a centrifuge tube 101 by using a pipette 100; in the second embodiment, the first metal nano material is the silver nanowires shown in fig. 6, the solvent is absolute ethyl alcohol (99.7 wt.%), the volume of the whole solution 102 is 300ul, the concentration is 10mg/ml, and the volume of the centrifugal tube 101 is 4 ml;
s1-2, transferring the second metal nano material solution 103 into a centrifugal tube 101 by using a pipette 100 to form a mixed solution 104 of the two metal nano materials; in the second embodiment, the second metal nano-material is the copper nanowire shown in fig. 3, the solvent is absolute ethyl alcohol (99.7 wt.%), the volume of the whole solution 103 is 300ul, and the concentration is 10 mg/m;
s1-3, adding the volatile solvent 105 into the centrifuge tube 101 by using a pipette 100 to form a mixed solution 106; in the second embodiment, a pipette 100 is used to add deionized water to the 4ml mark of the centrifuge tube 101;
s2, placing the centrifugal tube 101 in an ultrasonic cleaning machine 107 for ultrasonic treatment, wherein in the second embodiment, the ultrasonic power is set to be 100W, and the ultrasonic time is set to be 20 min;
s3-1, after the ultrasound is finished, taking out the centrifugal tube 101, and placing the centrifugal tube in a centrifuge 109 for centrifugation, wherein in the second embodiment, the centrifugation speed is 7000r/min, and the centrifugation time is 6 min;
s3-2, after the centrifugation is finished, removing the supernatant 110, and leaving the high-concentration metal nano slurry 111; in the second example, after centrifugation, 3.5ml of the supernatant was removed with a pipette;
s4, spin-coating the high-purity metal nano-slurry 111 on a substrate 112, in the second embodiment, setting the rotation speed of a spin-coating machine to be 500rad/min, setting the rotation time to be 25s, and setting the substrate 112 to be a metal aluminum sheet with a smooth surface and a roughness grade of less than 0.1;
s5, carrying out vacuum heating drying on the substrate 112, in the second embodiment, putting the substrate 112 into a vacuum drying oven, wherein the temperature of the drying oven is 45 ℃, the time is 10min, taking out the substrate 112 after the solvent is completely volatilized, and forming a dried metal nano mixed material 116 on the surface of the substrate 112;
s6-1, placing a light-transmitting sheet 115 on the substrate 112, passing the laser 114 through the light-transmitting sheet 115, and scanning the dried metal nano-hybrid material 116; in the second embodiment, a transparent glass plate is used as the light-transmitting plate 115, and is placed on the substrate 112 to press the metal nano-hybrid material 116; the adopted laser is nanosecond laser, the wavelength of the laser is 1064nm, the power of the laser is 250mW, the scanning speed is 1000mm/s, the diameter of a light spot is 78um, the pulse frequency of the laser is 20k, and the pulse width is 115 ns;
and S6-2, obtaining the nano alloy particles 117 after the laser 114 scanning is finished.
And (3) performance characterization:
as shown in fig. 7, as can be seen from the scanning electron microscope image, the diameter of the nano-alloy particles prepared in the second embodiment is 100nm to 800nm, and no obvious void exists on the surface. As shown in fig. 8, it was confirmed by energy spectrum analysis that the nano-alloy particles prepared in the second example contained two metal elements of silver and copper.
The above embodiments are merely illustrative of the technical solutions of the present invention. The laser-induced preparation method of the nano-alloy particles according to the present invention is not limited to the above embodiments, but is subject to the scope defined by the claims. Any modification or supplement or equivalent replacement made by a person skilled in the art on the basis of this embodiment is within the scope of the invention as claimed in the claims.
Claims (8)
1. A method for preparing nano alloy particles by laser induction is characterized by comprising the following steps:
step 1, adding at least two metal nano material solutions into a centrifugal tube, and adding a proper amount of volatile solvent to form a mixed solution;
step 2, ultrasonically mixing the solution to uniformly mix all the metal nano materials;
step 3, centrifugally concentrating the ultrasonic mixed solution to obtain nano slurry, wherein the centrifugal rotating speed of centrifugal concentration is 2000-15000 rad/min, the centrifugal time is 2-10 min, and the volume of the centrifuged nano slurry is 5-25% of the volume of the mixed solution;
step 4, spin-coating the nano-slurry on the substrate;
step 5, carrying out vacuum heating drying on the substrate after the spin coating is finished, and forming a drying coating layer on the surface of the substrate, wherein the temperature of the vacuum heating drying is 30-65 ℃, and the time is 5-1800 s;
and step 6, pressing the light-transmitting sheet on the surface of the substrate with the dry coating layer, and then scanning the metal nano material on the substrate by passing laser through the light-transmitting sheet to obtain the nano alloy particles, wherein the power of the laser is not lower than 220mW, the scanning speed of the laser is 20-2000 mm/s, and the diameter of a light spot is larger than 70 um.
2. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
in the step 1, the adopted metal nano material is at least one of metal nano particles and metal nano wire materials, the diameter of the metal nano particles is 10-600 nm, and the diameter of the metal nano wires is 10-800 nm.
3. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
wherein, in the step 1, the adopted volatile solvent is any one or a mixture of more of alcohols, ketones, benzenes, chloroform and deionized water.
4. The laser-induced preparation method of nano-alloy particles as set forth in claim 1, wherein:
in step 1, the ratio of the volume of the mixed solution to the volume of the metal nanomaterial solution is 3: 1-15: 1.
5. The laser-induced preparation method of nano-alloy particles as set forth in claim 1, wherein:
wherein in the step 2, the ultrasonic time is 5-40 min; the ultrasonic power is 80W-100W.
6. The laser-induced preparation method of nano-alloy particles as set forth in claim 1, wherein:
in step 4, the spin coating speed is 100rad/min to 6000rad/min, and the spin coating time is 5s to 60 s.
7. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
in step 4, the substrate is a metal substrate with a smooth and flat surface, and the surface roughness grade should be less than 0.1.
8. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
in step 6, the diameter of the light spot is larger than 70um and less than or equal to 200um, the pulse frequency of the laser is 10-200 k, the pulse width is 50 fs-200 ns, the wavelength of the laser is 248-1064 nm, and the power of the laser is 220-5000 mW.
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| CN105798447B (en) * | 2016-04-12 | 2018-06-29 | 苏州大学 | A kind of method and its application that metal nanometer line is prepared using nanometer interconnection |
| CN106041060B (en) * | 2016-05-31 | 2018-02-16 | 华中科技大学 | A kind of method for preparing nano composite material using laser welding in the liquid phase |
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