CN114210993A - Method for preparing hollow gold nanospheres by rapid sintering - Google Patents
Method for preparing hollow gold nanospheres by rapid sintering Download PDFInfo
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- CN114210993A CN114210993A CN202111556120.6A CN202111556120A CN114210993A CN 114210993 A CN114210993 A CN 114210993A CN 202111556120 A CN202111556120 A CN 202111556120A CN 114210993 A CN114210993 A CN 114210993A
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a method for preparing hollow gold nanospheres by rapid sintering. The method comprises the following specific processes: firstly, preparing gold nanoparticles and loading the gold nanoparticles on the surface of a substrate; and then, directly accessing the gold nanoparticles loaded on the substrate into a power supply or placing the gold nanoparticles on the surface of a heating medium accessed into the power supply, introducing instantaneous large current of 50-200A to two ends of the sample or the heating medium, rapidly heating the sample or the heating medium to 1400-2500K, and keeping heating for 5-60 seconds to enable gold atoms to diffuse to the outer surface to form a hollow structure. The method for preparing the hollow gold nanospheres by using the instantaneous large-current rapid heating sintering method is rapid and simple, has low cost, and the prepared hollow gold nanospheres have stable structures and high specific surface areas and have wide application prospects in the fields of biomedicine, optics, energy catalysis and the like.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a method for forming a hollow structure of gold nanoparticles by rapid sintering.
Background
The gold nanoparticles have unique surface structure, optical characteristics, stability and biocompatibility, so that the gold nanoparticles are widely applied to the fields of biomedicine, optics, energy catalysis and the like. The gold nanoparticles with hollow structures can realize the modulation of the characteristic absorption wavelength from a visible light region to a near infrared light region, and are beneficial to photo-thermal treatment of organisms. Meanwhile, the unique cavity of the hollow gold nanosphere is proved to have unique plasma and optical properties, and can absorb spectral red shift to form a photo-thermal conversion reagent. In addition, compared with solid gold particles, the hollow gold has higher specific surface area and lower noble metal content, so that the catalytic activity of the gold nanoparticles is improved, and the cost is reduced.
In order to obtain hollow nanostructures, a conventional method is a template method, in which a template is used as a core of a hollow sphere structure, a shell material is introduced on the surface of the template, and finally the core is removed to form an internal hollow structure. However, the template method involves final template removal, and on one hand, the operation procedure is complex, a sacrificial agent exists, and the cost is high; on the other hand, the microsphere structure is also damaged to a certain extent. In addition, there are liquid phase methods, high temperature dissolution methods, spraying methods, etc., but these methods usually involve various chemicals participating in the reaction, and introduce impurities, resulting in impure products. And the nano material can be agglomerated in a liquid phase, and the long-time high-temperature treatment can also cause the problems of particle growth and the like, which are not favorable for the application of the hollow nano gold. Therefore, a simple, fast and low-cost method for preparing high-purity hollow nano-gold is urgently needed to be found so as to promote the practical application of the hollow nano-gold in the fields of biomedicine, optics, energy catalysis and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing hollow gold nanospheres by rapid sintering.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing hollow gold nanospheres by rapid sintering comprises the following steps:
(1) preparing gold nanoparticles and loading the gold nanoparticles on a substrate;
(2) and (2) carrying out rapid heating treatment on the gold nanoparticles obtained in the step (1) by current.
Further, the specific process for preparing the gold nanoparticles loaded on the substrate in the step (1) comprises the following steps:
(a) adding a proper amount of base material into diethylene glycol, and stirring for dissolving;
(b) adding 0.1mmol of gold bromide into the solution (a), stirring for 30 minutes to dissolve, and adding a reducing agent with 1-2 times of stoichiometric ratio to reduce the gold bromide for 30 minutes;
(c) centrifuging the solution (b) at 8000 rpm, collecting precipitate, washing with n-hexane and acetonitrile solution for 3 times, and oven drying.
Further, the substrate in step (1) needs to have a high specific surface area.
Further, the substrate in the step (1) is one or more of carbon, silicon dioxide, graphene, carbon nanotubes, silicon carbide, silicon nitride and aluminum oxide.
Further, the loading amount of the gold nanoparticles in the step (1) on the substrate is 5% -50% by mass fraction.
Further, the reducing agent in the step (1) is one or more of lithium hydride, potassium hydride, sodium borohydride, sodium citrate and borane ammonia complex.
Further, the rapid temperature-raising treatment in the step (2) includes directly connecting the gold nanoparticles loaded on the substrate to a direct-current power supply for direct heating and placing the gold nanoparticles loaded on the substrate on a heating medium for indirect heating.
Further, the heating medium for the rapid temperature rise treatment in the step (2) includes one or more of a tungsten boat, a graphite boat, a carbon cloth, a nickel boat, a molybdenum boat, a tantalum boat, and titanium boride.
Further, the specific process of rapidly heating up and heating the gold nanoparticles in the step (2) is as follows:
(a) placing the gold nanoparticles loaded on the substrate on a heating medium with rapid temperature rise, or pressing the gold nanoparticles loaded on the substrate into a sheet for direct use;
(b) connecting a direct current power supply to two ends of the heating medium or the gold nanoparticle sheet loaded on the substrate;
(c) and (3) introducing 50-200A of current to two ends of the heating medium or the gold nanoparticle sheet loaded on the substrate to enable the surface of the sample to reach 1400-2500K, keeping for 5-60 seconds, and finally taking down the sample.
The method for preparing the hollow gold nanospheres by rapid sintering provided by the invention has the following advantages:
(1) the preparation time of the material is short, no new impurity is introduced, and the obtained product is pure;
(2) the prepared hollow gold nanosphere has a stable structure and a high specific surface area, and has a wide application prospect in the fields of biomedicine, optics, energy catalysis and the like;
(3) the preparation method is simple, low in cost and capable of realizing large-scale preparation.
Drawings
FIG. 1 is an X-ray diffraction pattern of carbon-supported gold nanoparticles prepared in example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of carbon-supported gold nanoparticles prepared according to example 1 of the present invention;
FIG. 3 is a distribution diagram of gold element of the hollow gold nanosphere prepared in example 1 under a transmission electron microscope according to the present invention;
FIG. 4 is a distribution diagram of gold element of the hollow gold nanospheres prepared in example 1 of the present invention under a transmission electron microscope by linear scanning;
FIG. 5 is an X-ray diffraction pattern of silica-supported gold nanoparticles prepared in example 2 of the present invention;
FIG. 6 is a distribution diagram of gold element of the hollow gold nanosphere prepared in example 2 of the present invention under a transmission electron microscope.
Detailed Description
The following description of the embodiments of the present invention is provided to facilitate the understanding of the present invention by those skilled in the art, but it should be understood that the present invention is not limited to the scope of the embodiments, and it will be apparent to those skilled in the art that various changes may be made without departing from the spirit and scope of the invention as defined and defined in the appended claims, and all matters produced by the invention using the inventive concept are protected.
Example 1
A method for preparing hollow gold nanospheres by rapid sintering comprises the following steps:
(1) preparing gold nanoparticles and loading the gold nanoparticles on a carbon substrate, and specifically comprising the following steps:
(a) adding 60mg of Keqin carbon black into 30mL of diethylene glycol, and stirring for dissolving;
(b) adding 43.8mg of gold bromide into the solution (a), stirring for 30 minutes to dissolve, and then adding 0.5mL of lithium super hydride;
(c) centrifuging the solution (b) at 8000 rpm, collecting precipitate, washing with n-hexane and acetonitrile solution for 3 times, and oven drying.
(2) Carrying out rapid high-temperature treatment on the carbon-loaded gold nanoparticles obtained in the step (1), and specifically comprising the following steps:
(a) placing carbon-loaded gold nanoparticles on the surface of carbon cloth;
(b) connecting two ends of the carbon cloth to a direct current power supply;
(c) 100A current is introduced to the two ends of the carbon cloth, the surface of the gold nanoparticle loaded by the carbon rapidly reaches 1900K within 3 seconds, and the temperature is kept for 20 seconds at the temperature.
Example 2
A method for preparing hollow gold nanospheres by rapid sintering comprises the following steps:
(1) preparing gold nanoparticles and loading the gold nanoparticles on a silicon dioxide substrate, and specifically comprising the following steps:
(a) adding 60mg of SBA-15 type silicon oxide into 30mL of diethylene glycol, and stirring for dissolving;
(b) adding 43.8mg of gold bromide into the solution (a), stirring for 30 minutes to dissolve, and then adding 0.5mL of lithium super hydride;
(c) centrifuging the solution (b) at 8000 rpm, collecting precipitate, washing with n-hexane and acetonitrile solution for 3 times, and oven drying.
(2) Carrying out rapid high-temperature treatment on the carbon-loaded gold nanoparticles obtained in the step (1), and specifically comprising the following steps:
(a) placing carbon-loaded gold nanoparticles on the surface of carbon cloth;
(b) connecting two ends of the carbon cloth to a direct current power supply;
(c) and (3) introducing 130A current to two ends of the carbon cloth, enabling the surface of the gold nanoparticle loaded with the carbon to rapidly reach 2100K within 3 seconds, and preserving the heat at the temperature for 20 seconds.
Example 3
A method for preparing hollow gold nanospheres by rapid sintering comprises the following steps:
(1) preparing gold nanoparticles and loading the gold nanoparticles on a carbon substrate, and specifically comprising the following steps:
(a) adding 60mg of Keqin carbon black into 30mL of diethylene glycol, and stirring for dissolving;
(b) adding 43.8mg of gold bromide into the solution (a), stirring for 30 minutes to dissolve, and then adding 0.5mL of lithium super hydride;
(c) centrifuging the solution (b) at 8000 rpm, collecting precipitate, washing with n-hexane and acetonitrile solution for 3 times, and oven drying.
(2) Carrying out rapid high-temperature treatment on the carbon-loaded gold nanoparticles obtained in the step (1), and specifically comprising the following steps:
(a) placing carbon-loaded gold nanoparticles on the surface of carbon cloth;
(b) connecting two ends of the carbon cloth to a direct current power supply;
(c) and (3) introducing 150A current to two ends of the carbon cloth, enabling the surface of the gold nanoparticle loaded with the carbon to rapidly reach 2200K within 3 seconds, and preserving the heat at the temperature for 10 seconds.
Example 4
A method for preparing hollow gold nanospheres by rapid sintering comprises the following steps:
(1) preparing gold nanoparticles and loading the gold nanoparticles on a carbon substrate, and specifically comprising the following steps:
(a) adding 80mg of Keqin carbon black into 30mL of diethylene glycol, and stirring for dissolving;
(b) adding 43.8mg of gold bromide into the solution (a), stirring for 30 minutes to dissolve, and then adding 0.5mL of lithium super hydride;
(c) centrifuging the solution (b) at 8000 rpm, collecting precipitate, washing with n-hexane and acetonitrile solution for 3 times, and oven drying.
(2) Carrying out rapid high-temperature treatment on the carbon-loaded gold nanoparticles obtained in the step (1), and specifically comprising the following steps:
(a) placing carbon-loaded gold nanoparticles on the surface of carbon cloth;
(b) connecting two ends of the carbon cloth to a direct current power supply;
(c) 100A current is introduced to the two ends of the carbon cloth, the surface of the gold nanoparticle loaded by the carbon rapidly reaches 1900K within 3 seconds, and the temperature is kept for 20 seconds at the temperature.
Claims (5)
1. A method for preparing hollow gold nanospheres by rapid sintering is characterized by comprising the following steps:
the method comprises the following steps: preparing gold nanoparticles and loading on a substrate:
adding a proper amount of base material into diethylene glycol, stirring for dissolving, adding 0.1mmol of gold bromide, stirring for dissolving again, adding a reducing agent with a stoichiometric ratio of 1-2 times that of the reducing agent to reduce the gold bromide, centrifuging at 8000 rpm, taking precipitate, washing with n-hexane and acetonitrile solution for 3 times respectively, and drying;
step two: rapidly heating the substrate-supported gold nanoparticles obtained in the step (1) to heat:
firstly, placing the gold nanoparticles loaded on the substrate on a heating medium which is heated rapidly, or pressing the gold nanoparticles loaded on the substrate into a sheet for direct use, then connecting a direct current power supply to two ends of the heating medium or the gold nanoparticle sheet loaded on the substrate, introducing instantaneous large current of 50-200A, enabling the surface of a sample to reach 1400-2500K, keeping the temperature for 5-60 seconds, and finally taking down the sample.
2. The method for preparing hollow gold nanospheres by rapid sintering according to claim 1, wherein the substrate material is one or more of carbon with high specific surface area, silicon dioxide, graphene, carbon nanotubes, silicon carbide, silicon nitride and aluminum oxide.
3. The method for preparing hollow gold nanospheres by rapid sintering according to claim 1, wherein the loading amount of the gold nanoparticles on the substrate is 5% -50% by mass fraction.
4. The method for preparing hollow gold nanospheres by rapid sintering according to claim 1, wherein the reducing agent is one or more of lithium super hydride, potassium super hydride, sodium borohydride, sodium citrate and borane ammonia complex.
5. The method for preparing hollow gold nanospheres by rapid sintering according to claim 1, wherein the heat-generating medium for rapid temperature rise treatment comprises one or more of tungsten boat, graphite boat, carbon cloth, nickel boat, molybdenum boat, tantalum boat and titanium boride.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115417441A (en) * | 2022-08-29 | 2022-12-02 | 兰州大学 | Method for preparing flaky nano barium fluoride by thermal decomposition method |
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| CN115417441B (en) * | 2022-08-29 | 2023-11-21 | 兰州大学 | Method for preparing flaky nano barium fluoride by thermal decomposition method |
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