Method for preparing nano alloy particles by laser induction
阅读说明:本技术 激光诱导制备纳米合金颗粒的方法 (Method for preparing nano alloy particles by laser induction ) 是由 周圣军 赵强 桂成群 陈东 万泽洪 于 2019-09-19 设计创作,主要内容包括:本发明提供了一种激光诱导制备纳米合金颗粒的方法,包括以下步骤:步骤1.将至少两种金属纳米材料溶液加入到离心管中,再添加适量的挥发性溶剂形成混合溶液;步骤2.超声混合溶液,使所有金属纳米材料混合均匀;步骤3.离心浓缩超声后的混合溶液,获得纳米浆料;步骤4.旋涂纳米浆料至基板上;步骤5.对旋涂完成后的基板进行真空加热干燥,在基板表面形成干燥涂覆层;步骤6.把透光片压在形成有干燥涂覆层的基板面上,然后激光穿过透光片扫描基板上的金属纳米材料,即可制得纳米合金颗粒,其中,激光的功率不低于220mW,光斑直径大于70um。本方法具有重复性好,生产速度快,效率高、耗时短,操作简单等优点。(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.)
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 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.
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 claimed 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 claimed in claim 1, wherein:
wherein, in the step 2, the ultrasonic time is 5min to 40 min; the ultrasonic power is 80W-100W.
6. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
wherein 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.
7. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
wherein, in the step 4, the spin coating speed is 100rad/min to 6000rad/min, and the spin coating time is 5s to 60 s.
8. 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.
9. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
wherein, in the step 5, the temperature of vacuum heating and drying is 30-65 ℃ and the time is 5-1800 s.
10. The laser-induced preparation method of nano-alloy particles as claimed in claim 1, wherein:
in step 6, the scanning speed of the laser is 20-2000 mm/s, the diameter of the 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 220-5000 mW.
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:
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in the
Preferably, the laser-induced preparation method of the nano-alloy particles provided by the invention can also have the following characteristics: in
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
s1-2, transferring the second metal
s1-3, adding the
s2, placing the
s3-1, after the ultrasonic treatment is finished, taking out the
s3-2, after the centrifugation is finished, removing the
s4, spin-coating the high-purity metal nano-
s5, carrying out vacuum heating drying on the
s6-1, placing a light-transmitting
and S6-2, obtaining the
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
s1-2, transferring the second metal
s1-3, adding the
s2, placing the
s3-1, after the ultrasound is finished, taking out the
s3-2, after the centrifugation is finished, removing the
s4, spin-coating the high-purity metal nano-
s5, carrying out vacuum heating drying on the
s6-1, placing a light-transmitting
and S6-2, obtaining the
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.
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