CN111822728B - Strawberry-shaped composite material and preparation method thereof - Google Patents

Strawberry-shaped composite material and preparation method thereof Download PDF

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CN111822728B
CN111822728B CN202010710197.3A CN202010710197A CN111822728B CN 111822728 B CN111822728 B CN 111822728B CN 202010710197 A CN202010710197 A CN 202010710197A CN 111822728 B CN111822728 B CN 111822728B
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strawberry
composite material
shaped composite
electrodes
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CN111822728A (en
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张昱
崔成强
王泽鹏
杨冠南
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Guangdong University of Technology
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Abstract

The invention relates to the technical field of nano materials, in particular to a strawberry-shaped composite material and a preparation method thereof. The preparation method comprises the steps of enabling a carrier gas source carrying core particles to enter a spark ablation device through electrodes, enabling the two electrodes to generate a spark ablation reaction under pulse voltage, ablating and evaporating surface materials of the two electrodes through high temperature generated by spark discharge, mixing the evaporated electrode materials with carrier gas, and rapidly depositing the mixture on the core particles to form the strawberry-shaped composite material. The preparation method is quick, simple and environment-friendly, can be used for continuous production, reduces the production cost and is beneficial to realizing industrial production; the prepared strawberry-shaped composite material has high purity, narrow particle size distribution and good dispersity, and the electrode nano particles on the strawberry-shaped composite material have uniform size and controllable size; by replacing the core particles and the electrode materials, different types of strawberry-shaped composite materials can be manufactured and can be applied to the fields of super-hydrophobic materials, self-cleaning coatings, solar cells, catalysis, biomedicine, electronics and the like.

Description

Strawberry-shaped composite material and preparation method thereof
Technical Field
The invention relates to the technical field of nano materials, in particular to a strawberry-shaped composite material and a preparation method thereof.
Background
Strawberry-like composite material refers to a novel material in which one material is discontinuously attached to the surface of another solid spherical particle. Due to the advantages of unique structure, high specific surface area, controllable surface property and the like of the strawberry-shaped composite material, great attention is paid to people. The strawberry-shaped composite material has a complex multi-layer structure, shows enhanced stability, special magnetism, unique optical properties and the like, and is widely applied to the fields of super-hydrophobic materials, self-cleaning coatings, solar cells, catalysis, biological medicines, electronics and the like.
At present, the methods for preparing the strawberry-shaped composite material mainly comprise a polymerization method and a self-assembly method, and specifically comprise a seed polymerization method, a micro-emulsion polymerization method, a soap-free emulsion polymerization method, an in-situ synthesis method, a template modification method, a chemical evaporation precipitation method, a layer-by-layer self-assembly method, a solution gel method, a direct synthesis method and other liquid-phase synthesis methods. However, the above preparation method has the following disadvantages: (1) Impurities are easily introduced in the preparation process, so that the purity of the prepared material is not high; (2) The aggregation of particles is easy to occur in the liquid phase reaction process, and the prepared composite material has poor dispersibility; (3) The preparation process is complicated, sometimes needs to use toxic and harmful chemical reagents, and is not environment-friendly. Due to the defects, the method has great limitation on industrial production.
Disclosure of Invention
The invention provides a strawberry-shaped composite material and a preparation method thereof, and solves the problems that the prepared strawberry-shaped composite material prepared by the existing preparation method of the strawberry-shaped composite material is low in purity, poor in dispersity, relatively complex in preparation process and toxic chemical reagents are used.
The specific technical scheme is as follows:
the invention provides a preparation method of a strawberry-shaped composite material, which is prepared by adopting a preparation system consisting of a carrier gas source, a spark ablation device and a collecting device which are connected in sequence, wherein two electrodes are symmetrically arranged on the left and right of the inner wall of the spark ablation device, the two electrodes are both in a hollow cylindrical shape, the axes of the two electrodes are positioned on the same horizontal straight line, and the carrier gas source, the two electrodes and the collecting device are communicated;
the preparation method comprises the following steps:
step 1: introducing the carrier gas source carrying the core particles into a spark ablation device through the electrode;
step 2: step 2: and applying pulse voltage to the two electrodes to perform spark ablation reaction, wherein the electrode material evaporated by spark ablation is deposited on the core particles to form the strawberry-shaped composite material.
Preferably, the carrier gas source is an inert gas and/or nitrogen.
Preferably, the flow rate of the carrier gas source is 0.1-30L/min.
Preferably, the particle size of the core particles is between 1nm and 100 μm.
Preferably, the core particles are selected from the group consisting of elemental metals, elemental metalloids, metallic compounds, inorganic non-metallic compounds or polymers;
the electrodes are selected from a conductor material or a semiconductor material.
Preferably, the elemental metal is selected from tin, cadmium, lead, zinc, antimony, magnesium, aluminum, germanium, silver, gold, copper, manganese, nickel, yttrium, iron, palladium, titanium, platinum, zirconium, chromium, vanadium, rhodium, molybdenum or tungsten;
the nonmetal simple substance is selected from boron, carbon or silicon;
the metal compound is selected from zinc oxide, nickel oxide, ferroferric oxide, manganese dioxide or barium titanate;
the inorganic non-metallic compound is selected from silicon dioxide or silicon carbide;
the polymer is selected from polyester, polycarbonate, polystyrene, polypropylene, polyvinylidene fluoride, polypyrrole or epoxy resin;
the conductor material is selected from tin, cadmium, lead, zinc, magnesium, aluminum, silver, gold, copper, manganese, nickel, yttrium, iron, palladium, titanium, platinum, zirconium, chromium, vanadium, rhodium, molybdenum, tungsten, carbon or ferroferric oxide;
the semiconductor material is selected from silicon, germanium, titanium dioxide, gallium arsenide, indium phosphide or silicon carbide.
Preferably, the inner diameter of the electrode is 1-100mm and the wall thickness is 1-10mm.
Preferably, the pulse voltage is 0.1-10kV, and the frequency is 1-200Hz.
The invention also provides a strawberry-shaped composite material, which is prepared by the preparation method;
the strawberry-like composite material includes a core particle and electrode nanoparticles discontinuously deposited on the core particle.
Preferably, the electrode nanoparticles have a particle size of 1 to 100nm.
According to the technical scheme, the invention has the following advantages:
the invention provides a preparation method of a strawberry-shaped composite material, which is based on a physical vapor deposition method of gas spark discharge.A carrier gas source carrying core particles enters a spark ablation device through electrodes, the two electrodes generate spark ablation reaction under pulse voltage, the carrier gas generates spark discharge under high-voltage pulse, the surface materials of the two electrodes are ablated and evaporated by high temperature generated by the discharge, and the evaporated electrode nano material is mixed with the carrier gas and deposited on the core particles to obtain the strawberry-shaped composite material.
The preparation method does not need to prepare a precursor, is quick, simple and environment-friendly in preparation, and can be used for continuous production, so that the production cost is reduced, and the industrialized large-scale production is facilitated; the strawberry-shaped composite material prepared by the preparation method has high purity, narrow particle size distribution and good dispersibility, and the electrode nano particles on the strawberry-shaped composite material have uniform size and controllable size; the preparation method can prepare different types of strawberry-shaped composite materials by replacing the materials of the core particles and the two electrodes, and can be widely applied to the fields of super-hydrophobic materials, self-cleaning coatings, solar cells, catalysis, biomedicine, electronics and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of a system for preparing a strawberry-shaped composite material according to an embodiment of the present invention;
wherein the illustration is as follows:
1. a spark ablation device; 2. an electrode; 3. and (4) a collecting device.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all of the embodiments. 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 embodiment of the invention provides a preparation method of a strawberry-shaped composite material, which is characterized in that a preparation system consisting of a carrier gas source, a spark erosion device and a collecting device which are connected in sequence is adopted for preparation, two electrodes are symmetrically arranged on the left and right of the inner wall of the spark erosion device, the two electrodes are both in a hollow cylindrical shape, the axes of the two electrodes are positioned on the same horizontal straight line, and the carrier gas source, the two electrodes and the collecting device are communicated.
In the preparation system provided by the embodiment of the invention, the spark ablation device is a closed container.
The carrier gas source is communicated with one of the electrodes through an air inlet pipeline, the other electrode is communicated with the collecting device through an air outlet pipeline and a deposition pipeline, one end of the deposition pipeline is communicated with the outlet end of the air outlet pipeline, and the other end of the deposition pipeline is positioned above the bearing substrate of the collecting device.
The installation axes of the air inlet pipeline and the air outlet pipeline are on the same horizontal straight line, and the installation axes of the air inlet pipeline and the air outlet pipeline are on the same horizontal straight line.
The air inlet pipeline is provided with a valve for controlling the flow rate of the carrier gas source.
In the embodiment of the invention, the distance between the two electrodes is 0.1-3 mm.
The preparation method of the strawberry-shaped composite material comprises the following steps:
step 1: a carrier gas source carrying core particles enters a spark ablation device through an electrode;
and 2, step: step 2: and applying pulse voltage to the two electrodes to perform spark ablation reaction, wherein the electrode material evaporated by spark ablation is deposited on the core particles to form the strawberry-shaped composite material.
In the embodiment of the invention, a carrier gas source carrying core particles enters a spark ablation device through a hollow cylindrical electrode in a direction parallel to the axis of the electrode through an air inlet pipeline, the two electrodes generate spark ablation reaction under pulse voltage, carrier gas generates spark discharge under high-voltage pulse, the carrier gas source is kept continuously introduced in the spark discharge process, the surface materials of the two electrodes are ablated and evaporated by high temperature generated by the discharge, the evaporated electrode material is mixed with the carrier gas, and then the mixture is rapidly deposited on the core particles to form electrode nano particles, so that the strawberry-shaped composite material is obtained. And keeping the continuous introduction of the carrier gas source during the rapid cooling process.
Further, the particle size of the core particles is 1nm-100 μm, and the average particle size is 20 nm-60 μm, so that the core particles are suspended in a carrier gas source and enter the spark ablation device in the form of aerosol.
Further, the carrier gas source is inert gas and/or nitrogen, wherein the inert gas is preferably argon and/or helium. According to the embodiment of the invention, the spark ablation reaction is carried out in the atmosphere of inert gas and/or nitrogen, so that the participation of active gas is avoided, and impurities are introduced, thereby improving the purity of the strawberry-shaped composite material. And continuously introducing a carrier gas source in the whole preparation process of the strawberry-shaped composite material.
Further, the flow rate of the carrier gas source is 0.1-30L/min. The embodiment of the invention can control the coverage rate of the electrode nano particles deposited on the strawberry-shaped composite material by controlling the flow of the carrier gas source, and is favorable for the uniform distribution of the electrode nano particles on the strawberry-shaped composite material under uniform airflow.
Further, the core particles are selected from a metal simple substance, a nonmetal simple substance, a metal compound, an inorganic nonmetal compound or a polymer, wherein the metal simple substance is selected from tin, cadmium, lead, zinc, antimony, magnesium, aluminum, germanium, silver, gold, copper, manganese, nickel, yttrium, iron, palladium, titanium, platinum, zirconium, chromium, vanadium, rhodium, molybdenum or tungsten, the nonmetal simple substance is selected from boron, carbon or silicon, the metal compound is selected from zinc oxide, nickel oxide, ferroferric oxide, manganese dioxide or barium titanate, and the polymer is selected from polyester, polycarbonate, polystyrene, polypropylene, polyvinylidene fluoride, polypyrrole or epoxy resin;
the electrode is selected from a conductor material or a semiconductor material, wherein the conductor material is selected from tin, cadmium, lead, zinc, magnesium, aluminum, silver, gold, copper, manganese, nickel, yttrium, iron, palladium, titanium, platinum, zirconium, chromium, vanadium, rhodium, molybdenum, tungsten, carbon or ferroferric oxide, and the semiconductor material is selected from silicon, germanium, titanium dioxide, gallium arsenide, indium phosphide or silicon carbide.
Furthermore, the inner diameter of the electrode is 1-100mm, preferably 5-50 mm, and the wall thickness is 1-10mm, preferably 2-10 mm;
in the present invention, the size of the electrode only affects the production efficiency of the material.
Further, the pulse voltage is 0.1 to 10kV, the frequency is 1 to 200Hz, preferably 0.7 to 5kV,20 to 150Hz.
In the embodiment of the invention, the size of the electrode nano-particles is adjusted by adjusting the size of the pulse voltage loaded on the electrode.
According to the preparation method of the strawberry-shaped composite material, a precursor does not need to be prepared, and the evaporated electrode material is directly deposited on the core particles based on a physical vapor deposition method of gas spark discharge to obtain the strawberry-shaped composite material; the strawberry-shaped composite material prepared by the preparation method has high purity, narrow particle size distribution and good dispersibility, and the electrode nano particles on the strawberry-shaped composite material have uniform size and controllable size; the preparation method can prepare different types of strawberry-shaped composite materials by replacing the materials of the core particles and the two electrodes, and can be widely applied to the fields of super-hydrophobic materials, self-cleaning coatings, solar cells, catalysis, biomedicine, electronics and the like.
The embodiment of the invention also provides a strawberry-shaped composite material prepared by the preparation method, and the strawberry-shaped composite material comprises core particles and electrode nano-particles discontinuously deposited on the core particles.
The particle size of the electrode nano-particles is 1-100nm, and the average particle size is 2-15 nm.
The strawberry-shaped composite material prepared by the embodiment of the invention has narrow particle size distribution, good dispersibility, uniform electrode nano particle size and uniform distribution on the surface of core particles.
Example 1
The preparation method of the barium titanate @ silver strawberry-shaped composite material comprises the following steps:
the method comprises the following steps: introducing nitrogen loaded with barium titanate particles with the particle size of 80nm into a spark ablation device at the flow rate of 2L/min;
step two: in the spark ablation device, a hollow cylindrical silver electrode with the inner diameter of 10mm and the wall thickness of 2mm is added with a pulse voltage of 0.3kV and 25Hz, and the surface materials of the two silver electrode materials are ablated and evaporated by high temperature generated in the spark discharge process;
the nano-silver particles produced by ablation are immediately deposited on the barium titanate core particles to form a barium titanate @ silver strawberry-like composite.
The average particle size of the core particle of the barium titanate @ silver strawberry-shaped composite particle prepared in the example is 80nm, and the average particle size of the electrode nanoparticle is 15nm and is uniformly distributed on the surface of the core particle.
Example 2
The preparation method of the silicon dioxide @ gold strawberry-shaped composite material comprises the following steps:
the method comprises the following steps: introducing helium gas loaded with silica particles with the particle size of 40nm into a spark ablation device at the flow rate of 0.5L/min;
step two: in the spark ablation device, a hollow cylindrical gold electrode with the inner diameter of 5mm and the wall thickness of 2mm is added with a pulse voltage of 0.7kV and 10.7Hz, and the surface material of the gold electrode material is ablated and evaporated at high temperature generated in the spark discharge process;
the nano-gold particles produced by ablation are immediately deposited onto the silica core particles to form a silica @ gold strawberry-like composite.
The average particle size of the core particle of the silica @ gold strawberry-shaped composite particle prepared in the example is 40nm, and the average particle size of the electrode nanoparticle is 10nm and is uniformly distributed on the surface of the core particle.
Example 3
The preparation method of the copper @ silver strawberry-shaped composite material comprises the following steps:
the method comprises the following steps: introducing nitrogen loaded with copper particles with the particle size of 30nm into a spark ablation device at the flow rate of 3L/min;
step two: in the spark ablation device, pulse voltage of 2kV and 150Hz is applied to a hollow cylindrical silver electrode with the inner diameter of 20mm and the wall thickness of 5mm, and high temperature is generated in the spark discharge process to ablate and evaporate the surface material of the silver electrode material;
the nano-silver particles produced by the ablation are immediately deposited onto the copper core particles to form a copper @ silver strawberry-like composite.
The average particle size of the core particles of the copper @ silver strawberry-shaped composite particles prepared in the embodiment is 30nm, and the average particle size of the electrode nanoparticles is 5nm and is uniformly distributed on the surfaces of the core particles.
Example 4
The preparation method of the polystyrene @ silicon strawberry-shaped composite material comprises the following steps:
the method comprises the following steps: introducing argon gas loaded with polystyrene particles with the particle size of 60 mu m into a spark ablation device at the flow rate of 3L/min;
step two: in the spark ablation device, pulse voltage of 4kV and 50Hz is applied to a hollow cylindrical silicon electrode with the inner diameter of 30mm and the wall thickness of 10mm, and high temperature is generated in the spark discharge process to ablate and evaporate the surface material of the silicon electrode material;
the nano-silicon particles produced by ablation are immediately deposited onto the polystyrene core particles to form a polystyrene @ silicon strawberry-like composite.
The polystyrene @ silicon strawberry-shaped composite particle prepared in this example had an average particle size of core particles of 60 μm, and the electrode nanoparticles had an average particle size of 2nm and were uniformly distributed on the surface of the core particles.
Example 5
The preparation method of the polypyrrole @ ferroferric oxide strawberry-shaped composite material comprises the following steps:
the method comprises the following steps: introducing nitrogen gas loaded with polypyrrole granules with the particle size of 50 mu m into a spark ablation device at the flow rate of 4L/min;
step two: in the spark ablation device, pulse voltage of 5kV and 20Hz is added to a hollow cylindrical ferroferric oxide electrode with the inner diameter of 50mm and the wall thickness of 10mm, and the surface material of the ferroferric oxide electrode material is ablated and evaporated by high temperature generated in the spark discharge process;
step three: and immediately depositing the nano ferroferric oxide particles generated by ablation on polypyrrole core particles to form the polypyrrole @ ferroferric oxide strawberry-shaped composite material.
The polypyrrole @ ferroferric oxide strawberry-shaped composite particles prepared in the embodiment have the average particle size of 50 μm of core particles, and the average particle size of electrode nanoparticles is 7nm and is uniformly distributed on the surfaces of the core particles.
Example 6
The preparation method of the carbon @ copper @ silver strawberry-shaped composite material comprises the following steps:
the method comprises the following steps: introducing nitrogen carrying carbon particles with the particle size of 40nm into a spark ablation device at the flow rate of 0.2L/min;
step two, in the spark ablation device, pulse voltage of 1kV and 25Hz is added on hollow cylindrical copper and silver electrodes with the inner diameter of 10mm and the wall thickness of 3mm, and the surface materials of the copper electrode and the silver electrode materials are ablated and evaporated by high temperature generated in the spark discharge process;
and step three, immediately depositing the nano-copper and nano-silver particles generated by ablation on the carbon core particles to form the carbon @ copper @ silver strawberry-shaped composite material.
The average particle size of the core particle of the carbon @ copper @ silver strawberry-shaped particle prepared in the example is 40nm, and the average particle size of the electrode nanoparticle is 3nm and is uniformly distributed on the surface of the core particle.
Example 7
The preparation method of the polyvinylidene fluoride @ aluminum magnesium alloy strawberry-shaped composite material comprises the following steps:
introducing nitrogen loaded with polyvinylidene fluoride particles with the particle size of 20nm into a spark ablation device at the flow rate of 1L/min;
step two, in the spark ablation device, pulse voltage of 2kV and 30Hz is added on a hollow cylindrical aluminum electrode and a magnesium electrode with the inner diameter of 15mm and the wall thickness of 3mm, and the surface materials of the aluminum electrode and the magnesium electrode are ablated and evaporated by high temperature generated in the spark discharge process;
and step three, immediately forming magnesium-aluminum alloy by the nano aluminum particles and the nano magnesium particles generated by ablation, and depositing the magnesium-aluminum alloy on polyvinylidene fluoride core particles to form the polyvinylidene fluoride @ aluminum-magnesium alloy strawberry-shaped composite material.
The average particle size of the core particle of the polyvinylidene fluoride @ aluminum magnesium alloy strawberry-shaped composite particle prepared by the embodiment is 20nm, and the average particle size of the electrode nano-particle is 2nm and is uniformly distributed on the surface of the core particle.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. The preparation method of the strawberry-shaped composite material is characterized by comprising the steps of preparing by using a preparation system consisting of a carrier gas source, a spark ablation device and a collecting device which are sequentially connected, wherein two electrodes are symmetrically arranged on the left and right of the inner wall of the spark ablation device, the two electrodes are both in a hollow cylindrical shape, the axes of the two electrodes are positioned on the same horizontal straight line, and the carrier gas source, the two electrodes and the collecting device are communicated;
the preparation method comprises the following steps:
step 1: introducing the carrier gas source carrying the core particles into the spark ablation device through the electrode;
step 2: applying a pulsed voltage to both of said electrodes to perform a spark-ablation reaction, said spark-ablated evaporated electrode material being deposited on said core particles to form a strawberry-like composite material.
2. The method according to claim 1, wherein the carrier gas source is an inert gas and/or nitrogen.
3. The production method according to claim 1, wherein the flow rate of the carrier gas source gas is 0.1 to 30L/min.
4. The method of claim 1, wherein the core particle has a particle size of 1nm to 100 μm.
5. The method of claim 1, wherein the core particle is selected from an elemental metal, an elemental nonmetal, a metal compound, an inorganic nonmetal compound, or a polymer;
the electrodes are selected from a conductor material or a semiconductor material.
6. The method according to claim 5, wherein the elemental metal is selected from tin, cadmium, lead, zinc, antimony, magnesium, aluminum, germanium, silver, gold, copper, manganese, nickel, yttrium, iron, palladium, titanium, platinum, zirconium, chromium, vanadium, rhodium, molybdenum, or tungsten;
the nonmetal simple substance is selected from boron, carbon or silicon;
the metal compound is selected from zinc oxide, nickel oxide, ferroferric oxide, manganese dioxide or barium titanate;
the inorganic non-metallic compound is selected from silicon dioxide or silicon carbide;
the polymer is selected from polyester, polycarbonate, polystyrene, polypropylene, polyvinylidene fluoride, polypyrrole or epoxy resin;
the conductor material is selected from tin, cadmium, lead, zinc, magnesium, aluminum, silver, gold, copper, manganese, nickel, yttrium, iron, palladium, titanium, platinum, zirconium, chromium, vanadium, rhodium, molybdenum, tungsten, carbon or ferroferric oxide;
the semiconductor material is selected from silicon, germanium, titanium dioxide, gallium arsenide, indium phosphide or silicon carbide.
7. The method of claim 1, wherein the electrode has an inner diameter of 1 to 100mm and a wall thickness of 1 to 10mm.
8. The method according to claim 1, wherein the pulse voltage is 0.1 to 10kV and the frequency is 1 to 200Hz.
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