CN113909486B - Preparation method of ferroferric oxide loaded carbon-based thin film gold nanocomposite particles - Google Patents

Preparation method of ferroferric oxide loaded carbon-based thin film gold nanocomposite particles Download PDF

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CN113909486B
CN113909486B CN202110839204.4A CN202110839204A CN113909486B CN 113909486 B CN113909486 B CN 113909486B CN 202110839204 A CN202110839204 A CN 202110839204A CN 113909486 B CN113909486 B CN 113909486B
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CN113909486A (en
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那伟丹
宋晓筱
欧昌金
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Xuzhou University of 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
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • 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
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
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    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide (Fe3O4)
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases
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    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties

Abstract

A preparation method of ferroferric oxide loaded carbon-based thin film gold nano composite particles. The problems of various morphology and poor stability of composite particles caused by loose nuclear and satellite structure and random satellite particle arrangement are solved. Selection of Fe 3 O 4 NPs and AuNPs serve as core structure particles and satellite particles, respectively. And carrying out surface carbon-based film formation on AuNPs by a hydrothermal method by taking sodium alginate as a carbon-based precursor to obtain AuNPs@CF. AuNPs@CF with Fe 3 O 4 NPs are subjected to hydrothermal reaction and CF is taken as a bridge to closely link the nuclear and sanitary particles to obtain the nuclear and sanitary structure composite nano particle-Fe 3 O 4 AuNPs@CF. The composite nano particles with stable core-shell structure, controllable satellite particle quantity and uniform distribution are obtained by introducing the carbon-based nano film and adopting a hydrothermal chemical bonding mode. Fe obtained in the present invention 3 O 4 AuNPs@CF has excellent superparamagnetism and SPR effects.

Description

Preparation method of ferroferric oxide loaded carbon-based thin film gold nanocomposite particles
Technical Field
The invention relates to the field of carbon-based thin-film gold nanoparticles, in particular to a preparation method of ferroferric oxide loaded carbon-based thin-film gold nanocomposite particles.
Background
With the continuous development of nano technology, single nano materials cannot completely meet the multiple requirements of people on materials. The composite material can comprehensively utilize the properties of each material, and concentrate various excellent properties on one construction unit. The ferroferric oxide nano particles have superparamagnetism due to the crystal structure and the composition components, and are often used for enriching an object to be detected in analysis and diagnosis so as to realize effective detection of ultra-low level large and small biomolecules in a clinical sample matrix. Gold nanoparticles have good optical absorption property and extremely high enhancement effect on signal intensity (Raman or fluorescence) due to the local plasmon resonance (SPR), and are widely applied to the fields of biosensing, tumor diagnosis and treatment. Gold nano-and ferroferric oxide as an inorganic material approved by the FDA has higher safety and environmental protection in the field of biological application. The ferroferric oxide/gold nano composite particles can be constructed to integrate superparamagnetism and local plasma resonance effects, and the application value of the ferroferric oxide/gold nano composite particles is far more than that of a single component. The core-wei ferroferric oxide/gold nano composite particle is a common structure with large specific surface area. The surface adsorption bonding or covalent bond stable bonding can be performed between the core particles and the satellite particles through electrostatic action, and the satellite particles are grown on the core surface in situ to form the composite particles. Wherein the nuclear guard particles obtained by electrostatic attraction are a loose composition form, and the structure is easy to open or form other structural systems in complex detection and diagnosis systems. Nanoparticles grown by in situ reactions on the surface of the core are difficult to maintain uniformity in size and a controlled distribution of number. The core-shell structure obtained by covalent bonding forms exhibits strong structural stability but there is still a difficulty in controlling the uniformity distribution of satellite particles and occurs with aggregation precipitation phenomenon of gold nano-materials during chemical bonding. And finally, developing a novel covalent bond construction mode to obtain the multifunctional ferroferric oxide/gold nano composite particle unit with controllable satellite quantity and high consistency in morphology, and the multifunctional ferroferric oxide/gold nano composite particle unit has potential application value for effectively enriching target objects, detecting the target objects with high sensitivity, analyzing the target objects in multiple modes and other related fields.
Disclosure of Invention
The invention aims to solve the problem of Fe with the existing core-shell structure 3 O 4 The composite material of AuNPs has single synthesis mode, and the obtained core-shell structure has large and stable morphology differenceInsufficient qualitative and the like. In order to solve the problems, the invention provides a preparation method of ferroferric oxide loaded carbon-based thin film gold nanocomposite particles; coating AuNPs with carbon-based nano film (CF), and taking CF as bridge and Fe as kernel 3 O 4 NPs are chemically bonded and a structurally stable and highly uniform core Wei Fuge particle is built by means of a vigorous hydrothermal reaction. The above materials inherit and integrate their own excellent physicochemical properties (superparamagnetism and SPR effect). In addition, the invention provides a method for synthesizing the carbon-based thin film gold nanoparticles.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
preparation method of ferroferric oxide loaded carbon-based thin film gold nano composite particles comprises the steps of firstly synthesizing superparamagnetism Fe 3 O 4 NPs and AuNPs serve as a loading base (or core structure) and satellite particles, respectively; performing surface carbon-based filming on AuNPs by using sodium alginate as a carbon-based precursor by adopting a hydrothermal method to obtain AuNPs@CF with controllable carbon-based nano film thickness; finally AuNPs@CF with Fe 3 O 4 NPs are placed in a hydrothermal reaction kettle, and CF is used as a bridge to closely link nuclear and guarding particles at the optimal temperature and time to obtain Fe 3 O 4 -AuNPs@CF。
Further, the preparation method comprises the following steps:
(1) Preparation of superparamagnetic iron Fe 3 O 4 NPs and AuNPs;
(2) Adding sodium alginate into gold nanoparticle solution, and magnetically stirring at room temperature to obtain a reaction solution;
(3) Transferring the reaction solution into a hydrothermal reaction kettle to perform hydrothermal reaction at different temperatures and times to obtain carbon-based nano films (CF) gold nanoparticles AuNPs@CF with different thicknesses;
(4) Combining AuNPs@CF solution with Fe 3 O 4 The NPs solution is uniformly mixed by mediation and is transferred into a hydrothermal reaction kettle for hydrothermal reaction;
(6) Separating and washing the target object by adopting a magnet to obtain the composite nano particle-Fe with a nuclear-sanitation structure 3 O 4 -AuNPs@CF。
Further; the adopted satellite particles are carbon-based thin film gold nanoparticles-AuNPs@CF, and specifically comprise the following components:
(1) Dissolving sodium alginate in the prepared gold nano solution, magnetically stirring and mixing for 0.5h at room temperature, and transferring into a hydrothermal reaction kettle with a polytetrafluoroethylene inner core;
(2) Reacting for 2-10 h at 160-220 ℃; the reaction product is obtained.
Further, the preparation of carbon-based nano-membranized gold nano-particles-AuNPs@CF with different thicknesses comprises the following steps:
(1) The hydrothermal reaction temperature is 180 ℃, the reaction time is 2 hours, and the ratio of the mass of the adopted carbon-based precursor sodium alginate to the volume of the AuNPs solution is (10-60 mg) 20mL;
(2) Sodium alginate in an amount of 20mg,20mL AuNPs solution, 0.325. 0.325mg/mL -1 The reaction is carried out at different temperatures of 160, 180, 200 and 220 ℃ for 2 hours;
(3) Sodium alginate in an amount of 60mg,20mL of AuNPs solution, 0.325 mg/mL) was subjected to hydrothermal synthesis at 220 ℃ at reaction times of 5h and 10h, respectively.
Further, the nuclear sanitation structure Fe 3 O 4 Preparation of AuNPs@CF, specifically: fe (Fe) 3 O 4 The NPs solution and the prepared AuNPs@CF solution are fully and uniformly mixed at room temperature by vortex; transferring the mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a high-temperature oven, and performing hydrothermal reaction to obtain the Fe with the nuclear-sanitary structure 3 O 4 -AuNPs@CF。
Further, the adjustable synthesis of the satellite number is specifically: fe (Fe) 3 O 4 NPs solution, 10mL,1.0mg/mL, and prepared 10mL AuNPs@CF concentrations were 1,2,4,8,16mg/mL, respectively -1 Is mixed fully and uniformly by vortex at room temperature; transferring into a hydrothermal reaction kettle, putting into a high-temperature oven, and reacting for 3 hours at 200 ℃; naturally cooling the reaction to room temperature, separating by using a magnet, washing for 3 times by using pure water and ethanol respectively, and freeze-drying for later use.
Further, fe obtained by hydrothermal reaction and by means of CF bridging construction mode 3 O 4 -AuNPs@The CF structure has strong stability, even satellite particle distribution, simple method and easy operation, and integrates superparamagnetism and SPR effect into one unit.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, in the existing mode of directly connecting the particles corresponding to the cores and the sanitation, the satellite particles are coated by adopting a carbon-based nano film (CF), and then the core particles and the satellite particles are connected by taking the CF as a bridge. The number of the satellite particles in the composite particles with the nuclear and guarding structures can be effectively controlled; hydrothermal is more intense than the stirring adopted in the prior art, so that the distribution of the satellite particle height uniformity can be realized. The introduction of the carbon-based nano film endows gold nano particles and the whole nuclear-guard structure with protection from nonspecific aggregation, can ensure the high stability of the whole structure in a complex biological environment, and avoids ligand exchange of sulfhydryl molecules on the surfaces of AuNPs in the structure. The invention obtains the composite nano particles with stable core-shell structure, controllable satellite (AuNPs@CF) quantity and uniform distribution through the introduction of the carbon-based nano film and a hydrothermal chemical bonding mode. Fe obtained in the present invention 3 O 4 The AuNPs@CF has excellent superparamagnetism and simultaneously exhibits excellent SPR effect.
Drawings
FIG. 1 shows (a) Fe prepared by the present invention 3 O 4 NPs, (b) aunps@cf prepared in example 6, and (c) Fe prepared in example 13 3 O 4 -a transmission electron microscope picture of aunps@cf;
FIG. 2 shows Fe prepared in example 13 3 O 4 -scanning electron microscope pictures of aunps@cf;
FIG. 3 is a diagram of Fe in the present invention 3 O 4 NPs, auNPs, auNPs@CF prepared in example 6 and Fe prepared in example 13 3 O 4 -ultraviolet absorption spectrum of aunps@cf.
FIG. 4 shows the Fe obtained in example 13 3 O 4 -magnetic saturation test pattern of aunps@cf.
FIG. 5 shows the Fe obtained in example 13 3 O 4 AuNPs@CF dark field imaging.
Fig. 6 is a schematic diagram of the technical scheme of the present invention.
Detailed Description
The technical scheme of the invention is further described in detail below with reference to the attached drawings and the detailed description: as shown in figures 1-6 of the drawings,
Fe 3 O 4 the preparation method of the NPs loaded AuNPs@CF composite particle comprises the following steps:
(1) Superparamagnetic Fe 3 O 4 Preparation of nanoparticles: fe (Fe) 3 O 4 The synthesis of NPs is described in the journal (Angew. Chem. Int. Ed.2009,48, 5875-5879). FeCl 3 (0.65 g,4.0 mmol) and sodium citrate (0.20 g,0.68 mmol) were dissolved in 20mL ethylene glycol. Thereafter, to FeCl 3 1.20g of sodium acetate is added into the sodium citrate-glycol system, stirred and reacted for 0.5h until the solution is uniform, transferred into a 50mL reaction kettle, reacted for 10h at 200 ℃, and cooled to room temperature. And finally, respectively washing with ethanol and water for 3 times, separating the magnetic nano particles by adopting a magnet, and finally, drying in a vacuum oven and collecting powder for later use.
(2) Preparation of AuNPs: 150. Mu.L, 0.1g/mL of HAuCl 4 The aqueous solution was dissolved in 150 mL deionized water. After the solution was heated to boiling by heating the jacket, sodium citrate solution (7.5 mL water +75.8 mg) was quickly injected into the solution and heating was continued until the solution turned reddish and no longer discoloured and the reaction stopped. The gold nanoparticles are put into a glass bottle for preservation, and put into a refrigerator with the temperature of 4 ℃ for cold storage.
(3) Gold nanoparticles (AuNPs@CF) coated with carbon-based nanomembranes of different thicknesses are prepared.
Test example 1: different masses (10, 20, 40, 60 mg) were weighed out [ corresponding to examples 1,2,3,4, respectively]20mL of prepared gold nano-particles (0.325 mg/mL) are added respectively -1 ) And (3) in the solution, magnetically stirring and mixing for 0.5h at room temperature, and transferring into a hydrothermal reaction kettle with a polytetrafluoroethylene inner core. Stopping the reaction after reacting for 2 hours at 180 ℃ and obtaining AuNPs@CF with the film thickness of 1,3,5 and 8nm respectively through subsequent purification treatment; under other conditions, the higher the mass concentration of the sodium alginate in a certain range is, the CF film is obtainedThe thicker the thickness.
Test example 2: 20mg of sodium alginate was added to 20mL of AuNPs (0.325. 0.325 mg/mL) solution, and after 2h of hydrothermal reaction at different reaction temperatures (160, 180, 200, 220 ℃ C.) [ corresponding to examples 5,6,7,8] respectively, the film thicknesses of the obtained AuNPs@CF were 2,3,5,10nm, respectively. Under other conditions, the higher the temperature, the thicker the film, within a certain temperature range, the more unchanged.
Test example 3: the amount of sodium alginate was 60mg, and the film thickness of AuNPs@CF obtained after purification was 12, 15nm at 220℃under hydrothermal reaction for 5h and 10h [ corresponding to examples 9, 10], respectively.
To sum up: the thickness of CF can be effectively regulated and controlled (1-15 nm) within a certain scale by regulating the amount of the carbon-based precursor, namely the amount of sodium alginate, the reaction time and the reaction temperature.
(4) Synthesis of aunps@cf (3 nm):
the synthesis conditions of experimental example 6 in experimental example 2 were selected to obtain aunps@cf having a carbon-based nanofilm thickness of 3nm by hydrothermal reaction. Firstly, 20mg of sodium alginate is weighed and dissolved in 20mL of prepared gold nano (0.325 mg/mL) -1 ) And (3) in the solution, magnetically stirring and mixing for 0.5h at room temperature, and transferring into a hydrothermal reaction kettle with a polytetrafluoroethylene inner core. The reaction was stopped after 2h at 180 ℃. After the solution was cooled to room temperature, it was centrifuged at 9000rpm/min for 10min, the centrifugation was repeated three times, and the precipitated fraction of AuNPs@CF was redissolved in water for further use.
(5) Different nuclear-to-sanitation ratios of Fe 3 O 4 Preparation of AuNPs@CF
Test example 4:10mL of Fe at 1.0mg/mL 3 O 4 NPs solution and 10mL AuNPs@CF (1, 2,4,8,16 mg/mL) prepared -1 ) [ corresponding to Experimental examples 11, 12, 13, 14, 15, respectively]The solution was thoroughly and homogeneously mixed by vortexing at room temperature. Then transferring the mixture into a hydrothermal reaction kettle, putting the mixture into a high-temperature oven, and reacting for 3 hours at 200 ℃. After the reaction is naturally cooled to room temperature, a magnet is adopted to separate and wash the target object, thus obtaining the nuclear-sanitation composite nano particle-Fe 3 O 4 AuNPs@CF. By hydrothermal sealingFe obtained by core-shell structure construction of CF bridge mode 3 O 4 The AuNPs@CF has strong structural stability and uniform satellite particle distribution.
Test example 5: the nuclear sanitation composite nano particle-Fe obtained by the invention 3 O 4 AuNPs@CF inherits superparamagnetic and SPR effects. The invention adopts a simple construction form and is easy to operate, and superparamagnetism and SPR effect are integrated into one unit.
FIG. 1a is 200nm Fe 3 O 4 And a Transmission Electron Microscope (TEM) of the NPs, and the material is used as a nuclear particle structure in a nuclear-sanitation composite structure. FIG. 1b is AuNPs@CF obtained in example 6, the thickness of the CF being 3nm.1c is Fe obtained in example 13 3 O 4 TEM image of AuNPs@CF composite nanoparticle, fe as a core structure can be seen by planar display of TEM 3 O 4 The surface of the composite particles is uniformly connected with AuNPs@CF, the structural difference between the composite particles is small, and the satellite particles are uniformly distributed.
FIG. 2 is Fe 3 O 4 Scanning Electron Microscope (SEM) pictures of AuNPs@CF (example 13), and the SEM shows that the composite material obtained by the nuclear sanitation construction method of the CF regulation bridging mode under the hydrothermal reaction condition has stable and uniform loading performance in a three-dimensional scale. Superparamagnetic Fe 3 O 4 NPs are used as a substrate, a large amount of AuNPs@CF can be loaded, and the specific surface area of the material is greatly improved by the structure.
FIG. 3 is Fe 3 O 4 NPs (420 nm), auNPs (520 nm), auNPs@CF (538 nm) and Fe 3 O 4 -uv absorbance spectrum of aunps@cf (445, 535 nm). Compared with gold nanoparticles, the carbon-based thin-film gold nanoparticles have the advantage that the maximum absorption spectrum of the carbon-based thin-film gold nanoparticles is subjected to red shift. Fe of nuclear sanitation structure 3 O 4 The ultraviolet absorption spectrum of AuNPs@CF has two absorption peaks, and a certain distance is formed between the two absorption peaks and the peak position of the core Wei Tezheng, so that the two absorption peaks are fused.
FIG. 4 shows the Fe obtained in example 13 3 O 4 Magnetic force curve test is carried out on AuNPs@CF, and the obtained magnetic saturation is 38.57emu g -1 With Fe 3 O 4 Magnetic saturation of NPsDegree of harmony (36.29 emu g) -1 ) In contrast, the values are close. The magnetic saturation data show that the nuclear-sanitation composite material keeps and inherits superparamagnetism, and is favorable for the synthesis and separation of the material and the separation and enrichment of a target object.
FIG. 5 shows the Fe obtained in example 13 3 O 4 Dark field microscopic imaging (DFM) experiments were performed with aunps@cf solution, and DFM results indicated that the core-guard composite nanoparticles were the strongest in yellow-green light scattering ability and exhibited high contrast to the background as if a starlike sky in the night. This phenomenon is related to the plasma absorption spectrum around 535nm in FIG. three, indicating that the core-guard composite nanoparticle has excellent SPR effect.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any changes or substitutions that do not undergo the inventive effort should be construed as falling within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope defined by the claims.

Claims (4)

1. Preparation method of ferroferric oxide loaded carbon-based thin film gold nano composite particles comprises the steps of firstly synthesizing superparamagnetism Fe 3 O 4 NPs and AuNPs serve as a core structure and satellite particles, respectively; the method is characterized in that sodium alginate is used as a carbon-based precursor, and a hydrothermal method is adopted to carry out surface carbon-based filming on AuNPs to obtain AuNPs@CF with controllable carbon-based nano film thickness; finally AuNPs@CF with Fe 3 O 4 NPs are placed in a hydrothermal reaction kettle to react for 3 hours at 200 ℃, and CF is taken as a bridge to lead Fe 3 O 4 Close linking of NPs and AuNPs to obtain Fe 3 O 4 -AuNPs@CF;
The method specifically comprises the following steps:
(1) Preparation of superparamagnetic iron Fe 3 O 4 NPs and AuNPs;
(2) Adding sodium alginate into gold nanoparticle solution, and magnetically stirring at room temperature to obtain a reaction solution;
(3) Transferring the reaction liquid into a hydrothermal reaction kettle to perform hydrothermal reaction at different temperatures and times to obtain carbon-based nano-film gold nanoparticles AuNPs@CF with different thicknesses;
(4) Combining AuNPs@CF solution with Fe 3 O 4 The NPs solution is uniformly mixed by vortex and transferred into a hydrothermal reaction kettle for hydrothermal reaction;
(5) Separating and washing the target object by adopting a magnet to obtain the composite nano particle-Fe with a nuclear-sanitation structure 3 O 4 -AuNPs@CF;
The adopted satellite particles are carbon-based nano-film gold nanoparticles-AuNPs@CF, and the preparation method specifically comprises the following steps:
(1) Dissolving sodium alginate in the prepared gold nano solution, magnetically stirring and mixing for 0.5h at room temperature, and transferring into a hydrothermal reaction kettle with a polytetrafluoroethylene inner core;
(2) Reacting for 2-10 h at 160-220 ℃; the reaction product AuNPs@CF is obtained.
2. The preparation method of the carbon-based nano-film gold nanoparticles-AuNPs@CF with different thicknesses is characterized in that:
(1) The hydrothermal reaction temperature is 180 ℃, the reaction time is 2 hours, and the ratio of the mass of the adopted carbon-based precursor sodium alginate to the volume of the AuNPs solution is (10-60 mg) 20mL;
(2) Sodium alginate in an amount of 20mg,20mL AuNPs solution, 0.325mg/mL -1 The reaction is carried out at different temperatures of 160, 180, 200 and 220 ℃ for 2 hours;
(3) The amount of sodium alginate was 60mg,20mL of AuNPs solution, 0.325mg/mL was subjected to hydrothermal synthesis at 220℃with reaction times of 5h and 10h, respectively.
3. The method according to claim 1, wherein the core-guard structure composite nanoparticle-Fe 3 O 4 Preparation of AuNPs@CF, specifically: fe (Fe) 3 O 4 The NPs solution and the prepared AuNPs@CF solution are fully and uniformly mixed at room temperature by vortex; transferring the mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a high-temperature oven, and performing hydrothermal reaction to obtain the composite nano particle-Fe with the nuclear-sanitation structure 3 O 4 -AuNPs@CF。
4. A method according to claim 1 or 3, characterized in that the adjustable synthesis of the number of satellite particles, in particular: fe (Fe) 3 O 4 NPs solution, 10mL,1.0mg/mL, and prepared 10mL AuNPs@CF concentrations were 1,2,4,8,16mg/mL, respectively -1 Is mixed fully and uniformly by vortex at room temperature; transferring into a hydrothermal reaction kettle, and putting into a high-temperature oven; naturally cooling the reaction to room temperature, separating by using a magnet, washing for 3 times by using pure water and ethanol respectively, and freeze-drying for later use.
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Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101323022A (en) * 2008-07-11 2008-12-17 中山大学 Method for preparing gold magnetic core-shell nano-particle
CN101343083A (en) * 2008-05-15 2009-01-14 复旦大学 Magnetic carbon sphere of surface finished C8 alkyl chain, preparation and application thereof
CN102861921A (en) * 2011-07-08 2013-01-09 西南民族大学 Preparation method of core-shell magnetic/gold nano particles
CN103065751A (en) * 2011-10-19 2013-04-24 中国科学院宁波材料技术与工程研究所 Magnetic MFe2O4/C/M' compound and preparation method thereof using aniline small organic molecules as a carbon source
CN104174865A (en) * 2013-05-22 2014-12-03 南京大学 Carbon-wrapped polyhedron silver nano-particle and controllable self-assembly preparation method thereof
CN104495950A (en) * 2014-11-07 2015-04-08 聊城大学 Preparation method of carbon encapsulated magnetic C/Fe3O4 nano composite material and application thereof
CN106040307A (en) * 2016-06-06 2016-10-26 北京科技大学 Preparation method for synthesizing Fe3O4(PAA)@C-Au core-shell-structured microspheres with one-step hydrothermal method
CN106111211A (en) * 2016-06-25 2016-11-16 董晓 A kind of modified core shell structure Fe3o4/ C/TiO2the preparation method of composite
CN107068319A (en) * 2017-04-06 2017-08-18 浙江大学 A kind of preparation method of hydrophobic magnetic composite
CN108888766A (en) * 2018-07-21 2018-11-27 熊振 A kind of support type magnetic Nano golden shell microballoon and preparation method thereof
CN109133189A (en) * 2018-09-17 2019-01-04 河北工业大学 The preparation method of carbon coated ferriferrous oxide nanoshell supported nano-gold particle
CN110211758A (en) * 2019-06-14 2019-09-06 南宁师范大学 Ferroso-ferric oxide/gold nano composite particles preparation method
KR20200044328A (en) * 2018-10-19 2020-04-29 한국세라믹기술원 Manufacturing method of magnetic iron oxide-carbon composite
CN111437388A (en) * 2019-01-15 2020-07-24 上海大学 Gold-silver alloy nano material, preparation method and application thereof

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101343083A (en) * 2008-05-15 2009-01-14 复旦大学 Magnetic carbon sphere of surface finished C8 alkyl chain, preparation and application thereof
CN101323022A (en) * 2008-07-11 2008-12-17 中山大学 Method for preparing gold magnetic core-shell nano-particle
CN102861921A (en) * 2011-07-08 2013-01-09 西南民族大学 Preparation method of core-shell magnetic/gold nano particles
CN103065751A (en) * 2011-10-19 2013-04-24 中国科学院宁波材料技术与工程研究所 Magnetic MFe2O4/C/M' compound and preparation method thereof using aniline small organic molecules as a carbon source
CN104174865A (en) * 2013-05-22 2014-12-03 南京大学 Carbon-wrapped polyhedron silver nano-particle and controllable self-assembly preparation method thereof
CN104495950A (en) * 2014-11-07 2015-04-08 聊城大学 Preparation method of carbon encapsulated magnetic C/Fe3O4 nano composite material and application thereof
CN106040307A (en) * 2016-06-06 2016-10-26 北京科技大学 Preparation method for synthesizing Fe3O4(PAA)@C-Au core-shell-structured microspheres with one-step hydrothermal method
CN106111211A (en) * 2016-06-25 2016-11-16 董晓 A kind of modified core shell structure Fe3o4/ C/TiO2the preparation method of composite
CN107068319A (en) * 2017-04-06 2017-08-18 浙江大学 A kind of preparation method of hydrophobic magnetic composite
CN108888766A (en) * 2018-07-21 2018-11-27 熊振 A kind of support type magnetic Nano golden shell microballoon and preparation method thereof
CN109133189A (en) * 2018-09-17 2019-01-04 河北工业大学 The preparation method of carbon coated ferriferrous oxide nanoshell supported nano-gold particle
KR20200044328A (en) * 2018-10-19 2020-04-29 한국세라믹기술원 Manufacturing method of magnetic iron oxide-carbon composite
CN111437388A (en) * 2019-01-15 2020-07-24 上海大学 Gold-silver alloy nano material, preparation method and application thereof
CN110211758A (en) * 2019-06-14 2019-09-06 南宁师范大学 Ferroso-ferric oxide/gold nano composite particles preparation method

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