CN114833337B - Preparation method of spherical gallium-magnesium Janus particles - Google Patents
Preparation method of spherical gallium-magnesium Janus particles Download PDFInfo
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- CN114833337B CN114833337B CN202210364959.8A CN202210364959A CN114833337B CN 114833337 B CN114833337 B CN 114833337B CN 202210364959 A CN202210364959 A CN 202210364959A CN 114833337 B CN114833337 B CN 114833337B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/06—Aluminium; Calcium; Magnesium; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A preparation method of spherical gallium-magnesium Janes particles relates to the technical field of metal preparation. In order to solve the problems that the existing gallium aluminum and gallium zinc Janes micromotors can be used as bactericides, but the gallium aluminum micromotors contain a large amount of aluminum ions, and aluminum is extremely toxic; if the gallium-zinc Janes micromotor is used as a bactericide, the action can be generated only in an acidic environment; the two kinds of metal particles are harmful to human bodies when used. The gallium-magnesium particles can be manufactured by adopting the preparation method, the aluminum layer is deposited on the surface of the exposed magnesium ball by utilizing vacuum sputtering equipment in the second step, the aluminum layer is used as an adhesion layer, the surface of the magnesium ball can be coated with a layer of gallium, and the ratio of aluminum ions in the aluminum layer is small and can be ignored; therefore, the gallium-magnesium particles are nontoxic, can be used as a bactericide, react with water to generate a sterilizing effect when in use, do not need to be used in a specific environment, and do not cause harm to human bodies. The invention is applicable to the field of metal preparation.
Description
Technical Field
The invention relates to the technical field of metal preparation, in particular to a preparation method of spherical gallium-magnesium Janus particles.
Background
Magnesium has wide distribution, active chemical property, good biocompatibility and easy acquisition. The Janus structure can enable hydrogen bubbles to be generated on one side of the particles, so that the particles have motion characteristics, and the generated water-driven micron particles can effectively move in different biological media, so that the Janus structure has a great prospect in different biomedical or industrial applications.
Gallium is a liquid metal with a low melting point and a high boiling point. So far, the successful synthesis of gallium aluminum and gallium zinc Janus micro-motors is mainly based on the embrittlement characteristic of liquid metal. While gallium aluminum Janus micromotors can use the reaction of aluminum nuclei with water to generate a driving force, excess aluminum can produce some toxicity: chemical propellants are required for gallium zinc Janus micromotors to generate driving force. Both types of micromotors have certain limitations in their application. The magnesium particles can directly use water as fuel to generate hydrogen bubbles to propel its power, thereby eliminating the need for common toxic fuels.
In summary, the existing gallium aluminum and gallium zinc Janus micromotors can be used as a bactericide, but the gallium aluminum micromotor contains a large amount of aluminum ions, and excessive aluminum generated in use can generate certain toxicity; if the gallium-zinc Janus micromotor is used as a bactericide, the action can be generated only in an acidic environment; both kinds of metal particles are harmful to human body.
Disclosure of Invention
The invention aims to solve the problems that the existing gallium-aluminum and gallium-zinc Janus micromotors can be used as bactericides, but the gallium-aluminum micromotors contain a large amount of aluminum ions, and excessive aluminum generated in use can generate certain toxicity; if the gallium-zinc Janus micromotor is used as a bactericide, the action can be generated only in an acidic environment; the two kinds of metal particles are harmful to human bodies when used, and a preparation method of spherical gallium magnesium Janus particles is provided.
The invention relates to a preparation method of spherical gallium-magnesium Janus particles, which comprises the following specific steps:
dispersing magnesium metal particles on a glass slide to form a particle single layer;
depositing an aluminum layer on the surface of the exposed magnesium ball by using vacuum sputtering equipment, wherein the deposition process is carried out at room temperature;
dispersing liquid metal gallium on another glass sheet in the same mass; the two slides were then stored under compression at 80 ℃ for 2 hours, cooled to room temperature (25 ℃), and the slides were carefully separated;
step four, stripping gallium and magnesium Janus particles from the glass slide in the step three by using an ultrasonic method, and then collecting by centrifugation;
step five, washing the centrifugally collected particles for 3-5 times by using absolute ethyl alcohol and acetone solution alternately;
sixthly, observing the morphology of the micron particles through analysis of a Scanning Electron Microscope (SEM) and an energy dispersive X-ray spectrum (EDX);
further, the particle size of the magnesium metal particles in the first step is 25 +/-5 microns;
further, the time for carrying out precipitation in the second step is kept within 120 s;
further, the pressure of aluminum in the vacuum sputtering equipment in the second step is 2.5mTor;
further, the direct current power of the vacuum sputtering device in the second step is 200W;
further, the purity of the vacuum sputtering aluminum target of the vacuum sputtering equipment in the second step is 99.999 percent;
furthermore, in the third step, the metal gallium needs to be preheated to 40 ℃;
further, in the fifth step, the collected particles are washed for 4 times by using absolute ethyl alcohol and acetone solution alternately;
compared with the prior art, the invention has the following beneficial effects:
the invention overcomes the defects of the prior art, the gallium-magnesium Janus particles can be manufactured by adopting the preparation method, the aluminum layer is deposited on the surface of the exposed magnesium ball by utilizing vacuum sputtering equipment in the step two, the aluminum layer is used as an adhesion layer, the surface of the magnesium ball can be coated with a layer of gallium, and the proportion of aluminum ions in the aluminum layer is small and can be ignored; therefore, the gallium-magnesium Janus particles are non-toxic, and can be used as a bactericide, and can react with water to generate a sterilizing effect when being used, so that the gallium-magnesium Janus particles are not required to be used in a specific environment and cannot cause harm to a human body.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) of spherical gallium and magnesium Janus particles with a single diameter of 25 microns prepared by the preparation method of spherical gallium and magnesium Janus particles;
FIG. 2 is an energy dispersive x-ray spectroscopy (EDX) of spherical gallium and magnesium Janus particles with a single diameter of 25 microns prepared by the preparation method of the spherical gallium and magnesium Janus particles;
FIG. 3 is a Scanning Electron Microscope (SEM) of a plurality of spherical gallium-magnesium Janus particles prepared by the method for preparing spherical gallium-magnesium Janus particles of the present invention;
FIG. 4 is an energy dispersive x-ray spectroscopy (EDX) of a plurality of spherical gallium-magnesium Janus particles prepared by the method for preparing spherical gallium-magnesium Janus particles of the present invention;
FIG. 5 is a particle size statistical chart of spherical gallium and magnesium Janus particles prepared by the preparation method of spherical gallium and magnesium Janus particles;
wherein Panel A of FIG. 4 shows the detection of the signal of magnesium in a plurality of magnesium gallium particles; b, detecting the signal of aluminum element in a plurality of gallium-magnesium particles; the diagram C is the detection of gallium element signals in a plurality of gallium magnesium particles, and the detection signals of the gallium element signals are strongest at the same position of aluminum element; and the D picture is a layered image of gallium-magnesium particle gallium-magnesium-aluminum elements of a plurality of Janus structures.
Detailed Description
The first embodiment is as follows: the present embodiment is described with reference to fig. 1 to fig. 5, and a specific method of preparing spherical gallium-magnesium Janus microparticles according to the present embodiment is as follows:
step one, dispersing magnesium metal particles on a glass slide to form a particle monolayer;
depositing an aluminum layer on the surface of the exposed magnesium ball by using vacuum sputtering equipment, wherein the deposition process is carried out at room temperature;
dispersing liquid metal gallium on another glass sheet in the same mass; the two slides were then stored under compression at 80 ℃ for 2 hours, cooled to room temperature (25 ℃), and the slides were carefully separated;
step four, stripping gallium-magnesium Janus particles from the glass slide in the step three by using an ultrasonic method, and then collecting the gallium-magnesium Janus particles through centrifugation;
step five, washing the centrifugally collected particles for 3-5 times by using absolute ethyl alcohol and acetone solution alternately;
sixthly, observing the morphology of the micron particles through analysis of a Scanning Electron Microscope (SEM) and an energy dispersive X-ray spectrum (EDX);
according to the specific embodiment, a deposition method is combined with a micro-contact method, a complex process is not needed, the synthesis steps are simple, and spherical gallium-magnesium Janus particles with the required particle size are directly obtained; in the second step, vacuum sputtering equipment is utilized to deposit an aluminum layer on the surface of the exposed magnesium ball, the aluminum layer is used as an adhesion layer, the surface of the magnesium ball can be coated with a layer of gallium, and the proportion of aluminum ions in the aluminum layer is small and can be ignored; therefore, the gallium-magnesium Janus particles are non-toxic, and can be used as a bactericide, and can react with water to generate a sterilizing effect when being used, so that the gallium-magnesium Janus particles are not required to be used in a specific environment and cannot cause harm to a human body.
The second embodiment is as follows: the present embodiment will be described with reference to fig. 1 to 5, which is a further limitation of the production method according to the first embodiment, and the method for producing spherical gallium magnesium Janus fine particles according to the present embodiment is characterized in that the magnesium metal fine particles in the first step have a particle size of 25 ± 5 μm.
The third concrete implementation mode: the present embodiment is described with reference to fig. 1 to 5, and the present embodiment further defines the preparation method according to the first embodiment, and the time for performing the precipitation in the second step is kept within 120s in the preparation method of spherical gallium and magnesium Janus particles according to the present embodiment;
in the specific embodiment, the time for precipitation in the second step is kept within 120s, the deposited aluminum layer is used as an adhesion layer, the minimum value is taken within the range of ensuring the effect, the gallium can penetrate through the crystal boundary of the aluminum, and the 120s precipitation effect is better after comparison of multiple groups of experimental results.
The fourth concrete implementation mode: the present embodiment is described with reference to fig. 1 to 5, and the present embodiment is a further limitation of the preparation method according to the first embodiment, in the preparation method of spherical gallium magnesium Janus particles according to the present embodiment, the pressure of aluminum in the vacuum sputtering apparatus in the second step is 2.5mTor;
in this embodiment, the pressure of aluminum in the vacuum sputtering apparatus in the second step is set to 2.5mTor, and the pressure of aluminum is set to 2.5mTor, so that aluminum can be uniformly attached to the surface of the magnesium particles.
The fifth concrete implementation mode is as follows: the present embodiment is described with reference to fig. 1 to 5, and the present embodiment is a further limitation to the preparation method according to the first or fourth embodiment, and the method for preparing spherical gallium magnesium Janus particles according to the present embodiment is characterized in that the dc power of the vacuum sputtering apparatus in the second step is 200W;
the sixth specific implementation mode is as follows: the present embodiment is described with reference to fig. 1 to 5, and the present embodiment is a further limitation to the preparation method according to the first or fourth embodiment, and in the preparation method of spherical gallium-magnesium Janus microparticles according to the present embodiment, the purity of the vacuum sputtering aluminum target of the vacuum sputtering apparatus in the second step is 99.999%;
the seventh embodiment: the present embodiment is described with reference to fig. 1 to fig. 5, and the present embodiment is a further limitation to the preparation method of the first embodiment, and the preparation method of spherical gallium-magnesium Janus fine particles of the present embodiment needs to preheat gallium metal to 40 ℃;
the specific implementation mode is eight: the present embodiment is described with reference to fig. 1 to 5, and the present embodiment is a further limitation of the preparation method according to the first embodiment, and the preparation method of spherical gallium magnesium Janus fine particles according to the present embodiment includes a fifth step of washing the collected particles with an absolute ethyl alcohol and an acetone solution alternately for 4 times;
in the embodiment, the collected particles are alternately washed by absolute ethyl alcohol and isopropanol solution for 4 times in the fifth step, organic impurities except metal particles are removed by acetone, and finally the particles are stored in the absolute ethyl alcohol.
Claims (5)
1. A preparation method of spherical gallium-magnesium Janus particles is characterized by comprising the following steps: the specific method comprises the following steps:
step one, dispersing magnesium metal particles on a glass slide to form a particle monolayer;
depositing an aluminum layer on the surface of the exposed magnesium ball by using vacuum sputtering equipment, wherein the deposition process is carried out at room temperature, the pressure of aluminum in the vacuum sputtering equipment is 2.5mTor, the direct current power is 200W, and the deposition time is kept within 120 s;
dispersing liquid metal gallium on another glass sheet in the same mass; pressing the two slides together at 80 deg.C for 2 hr, cooling to room temperature of 25 deg.C, and separating the slides;
step four, stripping gallium-magnesium Janus particles from the glass slide in the step three by using an ultrasonic method, and then collecting the gallium-magnesium Janus particles through centrifugation;
step five, washing the centrifugally collected particles for 3-5 times by using absolute ethyl alcohol and acetone solution alternately;
and sixthly, observing the morphology of the micron particles through scanning electron microscope SEM and energy dispersive x-ray spectral EDX analysis.
2. The method for preparing spherical gallium-magnesium Janus particles according to claim 1, wherein the method comprises the following steps: the particle size of the magnesium metal particles in the first step is 25 +/-5 microns.
3. The method for preparing spherical gallium-magnesium Janus particles according to claim 1, wherein the method comprises the following steps: the purity of the vacuum sputtering aluminum target of the vacuum sputtering equipment in the step two is 99.999 percent.
4. The method for preparing spherical gallium-magnesium Janus particles according to claim 1, wherein the method comprises the following steps: in the third step, the metallic gallium needs to be preheated to 40 ℃.
5. The method for preparing spherical gallium-magnesium Janus particles according to claim 1, wherein the method comprises the following steps: in the fifth step, the collected particles are washed by using absolute ethyl alcohol and acetone solution for 4 times alternately.
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