CN111069625B - Preparation method of flaky platinum nanoparticles - Google Patents

Preparation method of flaky platinum nanoparticles Download PDF

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CN111069625B
CN111069625B CN202010009305.4A CN202010009305A CN111069625B CN 111069625 B CN111069625 B CN 111069625B CN 202010009305 A CN202010009305 A CN 202010009305A CN 111069625 B CN111069625 B CN 111069625B
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platinum
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CN111069625A (en
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胡劲
孙浩然
段云彪
王开军
张维钧
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Kunming University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0551Flake form nanoparticles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B22F2009/245Reduction reaction in an Ionic Liquid [IL]

Abstract

The invention relates to a preparation method of flaky platinum nano-particles, belonging to the technical field of precious metal nano-material preparation. Dissolving a platinum precursor in deionized water or absolute ethyl alcohol, and adjusting the pH value to 1-3 by using hydrochloric acid to obtain a platinum precursor solution; dropwise adding a reducing agent solution into a platinum precursor solution under the conditions of stirring at the temperature of 200-300 ℃ and an external electric field, and reacting until the pH value of the system is 6.5-7.5 to obtain a suspension; wherein the reducing agent is ethylene glycol; and (3) carrying out solid-liquid separation on the suspension, washing the solid by sequentially adopting absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain the flaky platinum nano-particles. The invention prepares the sheet platinum nano-particles with the size of tens of microns or hundreds of microns in a liquid phase reaction system, and the yield can reach more than 95 percent.

Description

Preparation method of flaky platinum nanoparticles
Technical Field
The invention relates to a preparation method of flaky platinum nano-particles, belonging to the technical field of precious metal nano-material preparation.
Background
Noble metal nanoparticles with different shapes have different physical and chemical properties such as electricity, optics, magnetism, catalysis and the like, and as nano materials of Pt group metals and alloys thereof are widely used as catalysts, in order to improve the catalytic performance of the noble metal nanoparticles, people try to regulate and control the shapes of the prepared Pt group noble metal nanoparticles, so far, people synthesize a series of Pt and alloy nano materials thereof with special shapes, such as Pt concave cubes, Pt nanowires, Pt-Pd alloy supercubes, Pt-Au octa-dendritic and octahedral nanocrystals, Pt-Ru alloy cubic frames and the like.
The flaky metal powder has good adhesive force, obvious shielding effect, strong light reflection capability and excellent conductivity, so that the flaky metal powder can be widely applied to the fields of slurry pigment or conductive material and the like.
However, synthesis of ultra-thin sheet-like platinum particles has not been achieved without a template, and it is particularly difficult to perform directional growth of nano-platinum particles if no template exists in the solution. The operation is complex, and the target product is not easy to obtain.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a template-free preparation method of flaky platinum nanoparticles, which adopts a liquid phase reduction method to prepare the flaky platinum nanoparticles, and retards the growth of a (001) crystal face in the growth process of the platinum nanoparticles through the intervention of an external electric field, so that the flaky growth of the whole nanoparticles along a two-dimensional plane is realized; the method can obtain the small-size sheet platinum nanoparticles with the size of tens of microns or hundreds of microns in a liquid-phase reaction system, and the yield of the platinum powder reaches more than 95 percent and is uniformly distributed; the reducing agent adopted by the method is common glycol, so that the preparation cost can be reduced, the flaky platinum nanoparticles of the product are easy to collect, and the yield of the platinum nanoparticles can be improved.
A preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor in deionized water or absolute ethyl alcohol, and adjusting the pH value to 1-3 by using hydrochloric acid to obtain a platinum precursor solution;
(2) dropwise adding a reducing agent solution into the platinum precursor solution obtained in the step (1) at the temperature of 200-300 ℃ under the conditions of stirring and external electric field, and reacting until the pH value of the system is 6.5-7.5 to obtain a suspension; wherein the reducing agent is ethylene glycol;
(3) and (3) carrying out solid-liquid separation on the suspension liquid obtained in the step (2), sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain the flaky platinum nanoparticles.
The concentration of the platinum precursor solution in the step (1) is 0.1-0.5 mol/L, and the platinum precursor is one or more of chloroplatinic acid, potassium chloroplatinate, ammonium chloroplatinate and potassium chloroplatinate.
The solvent of the reducing agent solution in the step (2) is deionized water or absolute ethyl alcohol, and the volume fraction of ethylene glycol in the reducing agent solution is 30-70%.
And (3) the voltage of an external electric field in the step (2) is 20-30V, and the frequency is 10-20 Hz.
The volume ratio of the reducing agent solution to the platinum precursor solution in the step (2) is 1-3: 1.
And (4) drying in vacuum in the step (3) at the temperature of 30-60 ℃.
The reaction mechanism is as follows: under the condition of no intervention of external environment, the growth rates of all low-index crystal faces of a face-centered cubic Pt unit cell are the same, the equilibrium shape of a substance liquid drop is determined by the minimum value of the surface energy of each crystal face, the vector length from the center of the crystal to the outer surface is in direct proportion to the surface free energy, in the growth process of a nano crystal, a high-energy crystal face is a crystal face with the growth rate obviously higher than that of a low-energy crystal face, so that the crystal face with the high growth rate disappears finally, the final shape is formed by the low-energy crystal face, the growth rates of different crystal faces are influenced, different shapes are obtained, and the surface energy of individual crystal faces can be reduced by the change of the external environment (an electric field, a magnetic field and the like) in the growth process of crystal grains, so that the effect of controlling the appearance is achieved; in the early stage of growth, the nano particles often rotate, the growth rate of the nano particles on each crystal face is the same, in the later development process, due to the intervention of an external electric field force, when the center distance of crystal grains is about 10 mu m from a {001} crystal face, the crystal faces stop growing, other crystal faces uniformly grow along the two-dimensional direction until the { reaches a limit position (10-100 mu m), and finally a sheet-shaped structure is formed.
The invention has the beneficial effects that:
(1) the surface energy of the nano-particles can be reduced through the action of an external electric field, so that the ligand mobility of the (001) crystal face is reduced, the growth of the crystal face is retarded, and other crystal faces grow freely, thereby realizing the flaky growth of the whole two-bit plane of the nano-particles;
(2) the invention adopts a magnetic stirrer, a simple alternating current power supply and other common laboratory instruments to carry out experiments under non-harsh conditions, and obtains flaky platinum particles with the size of tens of microns in a liquid phase reaction system by strictly controlling proper platinum ion concentration, proper surfactant and surfactant concentration, and proper reducing agent and reducing agent concentration, wherein the yield of platinum powder is more than 95% and the platinum powder is uniformly distributed.
Drawings
FIG. 1 is a scanning electron micrograph (magnification 2000 times) of the platelet-shaped platinum nanoparticles prepared in example 1;
FIG. 2 is a scanning electron micrograph (magnification 200 times) of the platelet-shaped platinum nanoparticles prepared in example 2;
FIG. 3 is a scanning electron micrograph (magnification 100 times) of the platelet-shaped platinum nanoparticles prepared in example 3;
FIG. 4 is a scanning electron micrograph (magnification 500 times) of the platelet-shaped platinum nanoparticles prepared in example 4;
FIG. 5 is an XRD spectrum of the tabular platinum nanoparticles prepared in examples 1-4.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (chloroplatinic acid) in absolute ethyl alcohol, and adjusting the pH value to 1 by adopting hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.1 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 30%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 20V, the frequency is 10Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 200 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 6.5 to obtain a suspension; wherein the volume ratio of the reducing agent solution (ethylene glycol solution) to the platinum precursor solution is 1.43: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotation speed of 5000r/min for 5min to separate solid from liquid, pumping out upper-layer liquid, sequentially washing the solid for 3 times by adopting absolute ethyl alcohol and deionized water, and performing vacuum drying at the temperature of 50 ℃ to obtain the flaky platinum nanoparticles;
the scanning electron microscope image (magnification 2000 times) of the sheet-shaped platinum nanoparticles of the embodiment is shown in fig. 1, and as can be seen from fig. 1, the platinum nanoparticles are sheet-shaped objects with the length of 30 micrometers and the width of about 20 micrometers, and have uniform appearance and uniform size;
the X-ray diffraction pattern of the sheet platinum nanoparticles in this example is shown in fig. 5, and from fig. 5 comparing Pt (JCPDS cardno.04-0802), the major crystal planes are (111), (220), and the platinum nanoparticles are in a face centered cubic structure, and according to the peak intensity comparison, it can be judged that these directions are all the preferred growth directions of the platinum particles.
Example 2: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (potassium chloroplatinate) in absolute ethyl alcohol, and adjusting the pH value to 3 by adopting hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.5 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 70%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 30V, the frequency is 20Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 300 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 7.5 to obtain a suspension; wherein the volume ratio of the reducing agent solution (ethylene glycol solution) to the platinum precursor solution is 3: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotation speed of 10000r/min for 10min to separate solid from liquid, pumping out upper-layer liquid, washing the solid for 3 times by sequentially adopting absolute ethyl alcohol and deionized water, and performing vacuum drying at the temperature of 80 ℃ to obtain the flaky platinum nanoparticles;
the scanning electron micrograph (magnification 200 times) of the platinum nanoparticles in the form of flakes is shown in fig. 2, and it can be seen from fig. 2 that the platinum nanoparticles are flakes having a size of about 300 μm;
the X-ray diffraction pattern of the sheet platinum nanoparticles in this example is shown in fig. 5, and from fig. 5 comparing Pt (JCPDS cardno.04-0802), the major crystal planes are (111), (220), and the platinum nanoparticles are in a face centered cubic structure, and according to the peak intensity comparison, it can be judged that these directions are all the preferred growth directions of the platinum particles.
Example 3: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (potassium chloroplatinite) in absolute ethyl alcohol, and adjusting the pH value to 2 by adopting hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.3 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 50%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 25V, the frequency is 15Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 250 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 7.0 to obtain a suspension; wherein the volume ratio of the reducing agent solution (glycol solution) to the platinum precursor solution is 2: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotating speed of 7500r/min for 8min to separate solid from liquid, pumping out the upper layer liquid, sequentially washing the solid with absolute ethyl alcohol and deionized water for 3 times, and vacuum-drying at 65 ℃ to obtain the sheet platinum nanoparticles;
in the present embodiment, a scanning electron microscope image (magnification 100 times) of the flaky platinum nanoparticles is shown in fig. 3, and it can be seen from fig. 3 that most of the platinum nanoparticles are flaky objects with a size of about 100 μm, and are uniformly distributed and uniform in shape;
the X-ray diffraction pattern of the sheet platinum nanoparticles in this example is shown in fig. 5, and from fig. 5 comparing Pt (JCPDS cardno.04-0802), the major crystal planes are (111), (220), and the platinum nanoparticles are in a face centered cubic structure, and according to the peak intensity comparison, it can be judged that these directions are all the preferred growth directions of the platinum particles.
Example 4: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (potassium chloroplatinite) in absolute ethyl alcohol, and adjusting the pH value to 1.5 by using hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.3 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 50%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 30V, the frequency is 10Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 200 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 6.7 to obtain a suspension; wherein the volume ratio of the reducing agent solution (ethylene glycol solution) to the platinum precursor solution is 3: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotation speed of 5000r/min for 10min to separate solid from liquid, pumping out upper-layer liquid, sequentially washing the solid for 3 times by adopting absolute ethyl alcohol and deionized water, and performing vacuum drying at the temperature of 80 ℃ to obtain the flaky platinum nanoparticles;
the scanning electron micrograph (magnification 100 times) of the platinum nanoparticles in the form of flakes is shown in fig. 4, and it can be seen from fig. 4 that the platinum nanoparticles are flakes with a size of about 100 μm;
the X-ray diffraction pattern of the sheet platinum nanoparticles in this example is shown in fig. 5, and from fig. 5 comparing Pt (JCPDS cardno.04-0802), the major crystal planes are (111), (220), and the platinum nanoparticles are in a face centered cubic structure, and according to the peak intensity comparison, it can be judged that these directions are all the preferred growth directions of the platinum particles.
Example 5: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (ammonium platinochloride and potassium platinochloride, wherein the molar ratio of the ammonium platinochloride to the potassium platinochloride is 1: 1) in absolute ethyl alcohol, and adjusting the pH value to 2.5 by using hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.5 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 60%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 20V, the frequency is 20Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 300 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 6.5 to obtain a suspension; wherein the volume ratio of the reducing agent solution (ethylene glycol solution) to the platinum precursor solution is 3: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotation speed of 10000r/min for 5min to separate solid from liquid, pumping out upper-layer liquid, sequentially washing the solid for 3 times by using absolute ethyl alcohol and deionized water, and performing vacuum drying at the temperature of 50 ℃ to obtain the flaky platinum nanoparticles;
in the scanning electron microscope image of the platinum nanoparticles in this example, the platinum nanoparticles are flakes with a size of about 80 μm.
Example 6: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (chloroplatinic acid and potassium chloroplatinate, wherein the molar ratio of the chloroplatinic acid to the potassium chloroplatinate is 2: 1) in absolute ethyl alcohol, and adjusting the pH value to 2.2 by using hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.2 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 40%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 22V, the frequency is 18Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 270 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 7.2 to obtain a suspension; wherein the volume ratio of the reducing agent solution (glycol solution) to the platinum precursor solution is 1: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotating speed of 7000r/min for 8min to separate solid from liquid, pumping out upper-layer liquid, sequentially washing the solid for 3 times by using absolute ethyl alcohol and deionized water, and performing vacuum drying at the temperature of 60 ℃ to obtain the flaky platinum nanoparticles;
in the scanning electron microscope image of the platinum nanoparticles in this example, the platinum nanoparticles are flakes with a size of about 80 μm.
Example 7: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (chloroplatinic acid and potassium chloroplatinite, wherein the molar ratio of the chloroplatinic acid to the potassium chloroplatinite is 1: 3) in deionized water, and adjusting the pH value to 2.8 by using hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.5 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 50%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 26V, the frequency is 16Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 230 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 7.0 to obtain a suspension; wherein the volume ratio of the reducing agent solution (glycol solution) to the platinum precursor solution is 1: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotating speed of 7000r/min for 5min to separate solid from liquid, pumping out upper-layer liquid, sequentially washing the solid for 3 times by using absolute ethyl alcohol and deionized water, and performing vacuum drying at the temperature of 70 ℃ to obtain the flaky platinum nanoparticles;
in the scanning electron microscope image of the platinum nanoparticles in this example, the platinum nanoparticles are flakes having a size of about 90 μm.
Example 8: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (chloroplatinic acid and ammonium chloroplatinite with the molar ratio of 3: 1) in deionized water, and adjusting the pH value to 2.5 by using hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.4 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 30%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 25V, the frequency is 10Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 250 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 6.9 to obtain a suspension; wherein the volume ratio of the reducing agent solution (ethylene glycol solution) to the platinum precursor solution is 3: 1;
(3) centrifuging the suspension obtained in the step (2) at the rotating speed of 7500r/min for 9min to separate solid from liquid, pumping out the upper layer liquid, sequentially washing the solid with absolute ethyl alcohol and deionized water for 3 times, and vacuum-drying at the temperature of 75 ℃ to obtain the flaky platinum nanoparticles;
in the scanning electron microscope image of the platinum nanoparticles in this example, the platinum nanoparticles are flakes having a size of about 90 μm.
Example 9: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (potassium chloroplatinate and potassium chloroplatinite with the molar ratio of 1: 1) in deionized water, and adjusting the pH value to 1.8 by using hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.3 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 70%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 24V, the frequency is 16Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) under the conditions of stirring at the temperature of 280 ℃ and an external electric field to react to generate platinum black until the pH value of the system is 7.2 to obtain a suspension; wherein the volume ratio of the reducing agent solution (ethylene glycol solution) to the platinum precursor solution is 3: 1;
(3) centrifuging the suspension obtained in the step (2) at a rotation speed of 5500r/min for 6min to separate solid from liquid, pumping out upper-layer liquid, sequentially washing the solid for 3 times by using absolute ethyl alcohol and deionized water, and performing vacuum drying at the temperature of 60 ℃ to obtain the flaky platinum nanoparticles;
in the scanning electron microscope image of the platinum nanoparticles in this example, the platinum nanoparticles are in the form of flakes with a size of about 85 μm.
Example 9: a preparation method of flaky platinum nanoparticles comprises the following specific steps:
(1) dissolving a platinum precursor (potassium chloroplatinate and ammonium chloroplatinite with the molar ratio of 1: 1) in deionized water, and adjusting the pH value to 1.2 by using hydrochloric acid to obtain a platinum precursor solution; wherein the concentration of the platinum precursor solution is 0.3 mol/L;
(2) dissolving ethylene glycol and absolute ethyl alcohol mutually to obtain a reducing agent solution, wherein the volume fraction of the ethylene glycol in the reducing agent solution is 60%, adhering copper sheets on two sides of a beaker filled with a platinum precursor solution, then connecting the beaker to a simple alternating current power supply, wherein the voltage is 28V, the frequency is 18Hz, and dropwise adding the reducing agent solution (the ethylene glycol solution) into the platinum precursor solution obtained in the step (1) to react and generate platinum black until the pH value of the system is 7.5 under the conditions of stirring at the temperature of 290 ℃ and an external electric field to obtain a suspension; wherein the volume ratio of the reducing agent solution (glycol solution) to the platinum precursor solution is 2: 1;
(3) centrifuging the suspension obtained in the step (2) at a rotation speed of 8000r/min for 10min to separate solid from liquid, removing upper-layer liquid, sequentially washing the solid with absolute ethyl alcohol and deionized water for 3 times, and vacuum drying at 80 ℃ to obtain flaky platinum nanoparticles;
in the scanning electron microscope image of the platinum nanoparticles in this example, the platinum nanoparticles are flakes with a size of about 80 μm.

Claims (5)

1. A preparation method of flaky platinum nanoparticles is characterized by comprising the following specific steps:
(1) dissolving a platinum precursor in deionized water or absolute ethyl alcohol, and adjusting the pH value to 1-3 by using hydrochloric acid to obtain a platinum precursor solution;
(2) dropwise adding a reducing agent solution into the platinum precursor solution obtained in the step (1) at the temperature of 200-300 ℃ under the conditions of stirring and external electric field, and reacting until the pH value of the system is 6.5-7.5 to obtain a suspension; wherein the reducing agent is ethylene glycol; wherein the voltage of the applied electric field is 20-30V, and the frequency is 10-20 Hz;
(3) and (3) carrying out solid-liquid separation on the suspension liquid obtained in the step (2), sequentially washing the solid with absolute ethyl alcohol and deionized water, and carrying out vacuum drying to obtain the flaky platinum nanoparticles.
2. The method for preparing the tabular platinum nanoparticles as claimed in claim 1, wherein: the concentration of the platinum precursor solution in the step (1) is 0.1-0.5 mol/L, and the platinum precursor is one or more of chloroplatinic acid, potassium chloroplatinate, ammonium chloroplatinite and potassium chloroplatinate.
3. The method for preparing the tabular platinum nanoparticles as claimed in claim 1, wherein: the solvent of the reducing agent solution in the step (2) is deionized water or absolute ethyl alcohol, and the volume fraction of ethylene glycol in the reducing agent solution is 30-70%.
4. The method for preparing the tabular platinum nanoparticles as claimed in claim 1, wherein: the volume ratio of the reducing agent solution to the platinum precursor solution in the step (2) is 1-3: 1.
5. The method for preparing the tabular platinum nanoparticles as claimed in claim 1, wherein: and (4) drying in vacuum in the step (3) at the temperature of 30-60 ℃.
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Publication number Priority date Publication date Assignee Title
CN106735302A (en) * 2016-12-30 2017-05-31 西安交通大学青岛研究院 A kind of preparation method of Pt nanowires

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CN102717090A (en) * 2011-03-31 2012-10-10 北京有色金属研究总院 Method for preparing ultrafine platinum powder by adopting liquid-phase reduction
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CN106975754B (en) * 2016-12-30 2019-08-30 杭州罗松贸易有限公司 A kind of preparation method of palladium nanometer wire
CN109261985A (en) * 2018-11-29 2019-01-25 韩金玲 A kind of preparation method of triangle Pt nanocrystal

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106735302A (en) * 2016-12-30 2017-05-31 西安交通大学青岛研究院 A kind of preparation method of Pt nanowires

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