CN105903948A - Gold nanoflower nano-particle and preparation method thereof - Google Patents

Gold nanoflower nano-particle and preparation method thereof Download PDF

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Publication number
CN105903948A
CN105903948A CN201610251906.XA CN201610251906A CN105903948A CN 105903948 A CN105903948 A CN 105903948A CN 201610251906 A CN201610251906 A CN 201610251906A CN 105903948 A CN105903948 A CN 105903948A
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nanoparticle
jenner
nano
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罗志辉
梁春杰
刘发
韦庆敏
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Yulin Normal University
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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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Eye Examination Apparatus (AREA)
  • Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)

Abstract

The invention discloses a gold nanoflower nano-particle and a preparation method thereof. A gold nano-particle prepared from gold nanoflowers through a sodium citrate reduction method serves as a seed, ethanol amine is added to reducing chloroauric acid, and accordingly the gold nanoflower nano-particle is obtained. By researching the synthesis conditions of gold nanostars, the gold nanoflower nano-particle is obtained through the reduction and preparation actions of the ethanol amine. Compared with a conventional nano-particle preparation method, the experiment method has the advantages that raw materials are easy to obtain, cost is low, operation is simple and fast, pollution is avoided, no surface active agent is needed, and controllability is good. The gold nanoflower nano-particle prepared through the method is provided with a rough surface, is of a flower-like (or branchlike) or other starlike structure, has excellent near-infrared absorbing capacity, and is suitable for being applied to the fields such as photo-thermal analysis, imaging analysis and sensors.

Description

A kind of Jenner's popped rice nanoparticle and preparation method thereof
Technical field
The invention belongs to nano material synthesis field, be specifically related to a kind of Jenner's popped rice nanoparticle and preparation method thereof.
Background technology
Nano material the most extensively paid close attention to by people because of the structure of its uniqueness and physicochemical property, especially noble metal nano particles Preparation and application.The catalytic property of noble metal nano particles, photoelectric property, at biology/chemical sensitisation and nonlinear optics and table The potential application of the aspect such as Raman scattering (SERS) that face strengthens makes it of increased attention.The character of nanoparticle is very Depending on their shapes and sizes in big degree, current people have been achieved for the biggest in terms of the controlledly synthesis of nanoparticle Progress.Coarse flower-shaped (or dendritic) nanoparticle of Current surface has the functions such as near-infrared Extinction Characteristic and photothermal deformation because of it to be made The research focus becoming biomedical boundary, near-infrared thermotherapy, near-infrared spectroscopy and the nano-scale gold particle of nano Au particle mediation Son has shown broad prospect of application as the research of pharmaceutical carrier.These nanoparticles have closely knit core and coarse feeler table Face.These nanoparticles on the one hand nano flower has bigger specific surface area, is preferable catalyst material;On the other hand nanometer The nanometer feeler on flower surface makes have a lot of focuses, all advantages characteristics of nano flower particle in same nanoparticle surface It is made to be pursued by the person of being engaged in scientific research.
The physicochemical properties unique in view of nanoparticle and composite thereof and huge using value, they will be cured at biology The numerous areas such as, sensor, photoelectric device and catalysis have broad application prospects.As the one of nano material, flower-shaped Nanometer gold, has character more special compared with other nano materials: the features such as fluorescence is strong, nontoxic, good water solubility.Flower-shaped Nanometer gold can be applied not only to the detection of the toxic ion such as mercury ion and cyanic acid ion, it is also possible at aspect necks such as sensing, imagings Also there is preferable application prospect in territory.Develop new method and technology prepares the flower-shaped golden nanometer particle of structure-controllable, function admirable And composite is for promoting rationale scientific research and practical application in industry to have great importance.
Exploring new synthetic route in practice, probe into problem crucial in micro-nano structure materials synthesis, exploitation nano material is respectively The particularly application development in life science in individual field, is one of the main contents of materials chemistry and life analysis and research. If the Effective Regulation of the structure of nano material, pattern and surface nature can be realized, manually cutting out of material property not only can be realized, The relation of material structure Yu performance can also be carried out the understanding that system is deep, this point to nano material at life analysis field Development has important practical significance.
Summary of the invention
For solving the problems referred to above, an object of the present invention is to provide a kind of Jenner's popped rice nanoparticle;The two of purpose are to provide this The preparation method of Jenner's popped rice nanoparticle.
The golden nanometer particle that the present invention prepares with reduction of sodium citrate method, as seed, reduces chlorine by adding different amounts of ethanolamine Auric acid, it is thus achieved that Jenner's popped rice nanoparticle, and the structure of material is explored with detection meanss such as ultraviolet, infrared, Electronic Speculum.
For solving to reach above-mentioned purpose, the present invention uses technical scheme in detail below:
A kind of Jenner's popped rice nanoparticle, it is characterised in that the surface of this nanoparticle is flower-like structure.
The preparation method of a kind of Jenner's popped rice nanoparticle, it is characterised in that comprise the following steps:
(1) preparation of golden nanometer particle seed:
First chlorauric acid solution added high purity water and carry out heating in water bath, adding sodium citrate solution, the color of solution by Colourless gradually redden, i.e. obtain red golden nanometer particle seed;
(2) preparation of Jenner's popped rice nanoparticle:
Take above-mentioned prepared golden nanometer particle seed and add high purity water, adding ethanolamine under water bath condition after magnetic agitation, adjust Joint pH, continues water-bath magnetic agitation, and solution colour is by light red purpling more blue through purplish blue complexion changed, finally gives gold nano Flower nanoparticle finished product.
Further, the concrete operations of above-mentioned steps (1) are: add 80-100ml high purity water and 200-500 μ l in three-neck flask Chlorauric acid solution, is placed in more than 90 DEG C water-baths, adds sodium citrate solution after 15~20min, and water-bath 60~90 DEG C Carrying out synthetic reaction, the color of solution is reddened gradually by colourless, terminates after 8-15 minute;By gained red nano gold seeds It is placed in closed glass container, in case next step prepares Jenner's popped rice nanoparticle.
Further, the concrete operations of above-mentioned steps (2) are: add Jenner's grain of rice in high purity water and step (1) in reaction bulb Sub-seed, under 15-30 DEG C of water-bath magnetic agitation 15~after 20 minutes add ethanolamine;Molten by dripping a small amount of sodium hydroxide Liquid regulation pH;Magnetic agitation in 40-70 DEG C of water-bath is proceeded to after 10-20 minute;After reaction 50-90min, the color of solution From light red purpling, blue through purplish blue complexion changed, finally give Jenner's popped rice nanoparticle finished product.
Further, in above-mentioned steps (1): the concentration of described gold chloride is 0.5-2wt%;The concentration of described sodium citrate is 0.5-1wt%.
Further, in above-mentioned steps (2), ethanolamine concentration is: 1000-2400 μ g/L, and volume is 500-2000 μ l;Jenner Rice corpuscles seed volume: 100-300 μ l;PH:6-12;Naoh concentration is 0.5-1.0mol/L;High purity water volume is 8-12mL.
Near-infrared thermotherapy, near-infrared spectroscopy and the nano Au particle of nano Au particle mediation is opened up as the research of pharmaceutical carrier Reveal broad prospect of application.Jenner's popped rice nanoparticle prepared by the present invention has the functions such as near-infrared Extinction Characteristic and photothermal deformation, Can be applied to develop biological sensor, nanometer sensor, catalyst nano element or nano electrochemical and related biological Field.
The invention have the benefit that the present invention, by studying the condition of synthesis gold nano star, is prepared with ethanolamine reduction Obtain Jenner's popped rice nanoparticle;This experimental technique for conventional nanoparticle preparation method, have raw material be easy to get, With low cost, simple and quick, pollution-free, without surfactant and the controllability advantage such as preferably.The gold nano that the present invention prepares Flower nanoparticle surface is coarse, for star topologies such as flower-shaped (or dendritic), has good near infrared absorption ability, is suitable for The fields such as photo-thermal is analyzed, imaging analysis, sensor use.
Accompanying drawing explanation
Fig. 1 is Jenner's popped rice nanoparticle ultraviolet spectrogram that in the present invention, embodiment 1-5 prepares;
Fig. 2 is Jenner's popped rice nanoparticle ultraviolet Electronic Speculum figure that in the present invention, embodiment 1 prepares.
Detailed description of the invention
Embodiment 1:
<1>preparation of golden nanometer particle seed
100mL high purity water and 500 μ L 2wt% chlorauric acid solutions are added, as more than 90 DEG C in 250mL three-neck flask In water-bath, adding 3mL 1wt% sodium citrate solution after 15~20min, the color of solution is reddened gradually by colourless, and Water-bath 90 DEG C carries out synthetic reaction, and after 15min, reaction terminates;Gained redness golden nanometer particle seed is placed in 100mL airtight In glass container, use in case next step prepares Jenner's popped rice nanoparticle;
<2>preparation of Jenner's popped rice nanoparticle
In the reaction bulb of 20mL, add 10mL high purity water, add the golden nanometer particle seed 100 μ L made in the first step, Magnetic agitation 15~to add 500 μ L concentration after 20 minutes be 1000 μ g/L ethanolamine under 25 DEG C of water-baths;By dropping 1.0 Mol/L sodium hydroxide solution regulation pH is 11, proceeds to magnetic agitation in 65 DEG C of water-baths after 20min, reacts 60min, molten The color of liquid is from light red purpling, blue through purplish blue complexion changed, it is thus achieved that Jenner's popped rice nanoparticle.
Embodiment 2:
<1>preparation of golden nanometer particle seed
80mL high purity water and 200 μ L 0.5wt% chlorauric acid solutions are added, as more than 90 DEG C in 250mL three-neck flask In water-bath, adding 6mL0.5wt% sodium citrate solution after 15~20min, the color of solution is reddened gradually by colourless, and Carrying out synthetic reaction water-bath 60 DEG C, after 10min, reaction terminates;Gained redness golden nanometer particle seed is placed in 100mL close Close in glass container, use in case next step prepares Jenner's popped rice nanoparticle;
<2>preparation of Jenner's popped rice nanoparticle
In the reaction bulb of 20mL, add 8mL high purity water, add the golden nanometer particle seed 150 μ L made in the first step, Magnetic agitation 15~to add 1000 μ L concentration after 20 minutes be 1500 μ g/L ethanolamine under 15 DEG C of water-baths;By dropping 0.5mol/L sodium hydroxide solution regulation pH is 8, proceeds to magnetic agitation in 40 DEG C of water-baths, react 50min after 10min, The color of solution is from light red purpling, blue through purplish blue complexion changed, it is thus achieved that Jenner's popped rice nanoparticle.
Embodiment 3:
<1>preparation of golden nanometer particle seed
90mL high purity water and 300 μ L1wt% chlorauric acid solutions are added, as more than 90 DEG C water in 250mL three-neck flask In bath, adding 5mL0.7wt% sodium citrate solution after 15~20min, the color of solution is reddened gradually by colourless, and Water-bath 70 DEG C carries out synthetic reaction, and after 12min, reaction terminates;Gained redness golden nanometer particle seed is placed in 100mL airtight In glass container, use in case next step prepares Jenner's popped rice nanoparticle;
<2>preparation of Jenner's popped rice nanoparticle
In the reaction bulb of 20mL, add 9mL high purity water, add the golden nanometer particle seed 200 μ L made in the first step, Magnetic agitation 15~to add 500 μ L concentration after 20 minutes be 2400 μ g/L ethanolamine under 30 DEG C of water-baths;By dropping 1mol/L Sodium hydroxide solution regulation pH is 9, proceeds to magnetic agitation in 60 DEG C of water-baths, react 70min, the face of solution after 12min Color is from light red purpling, blue through purplish blue complexion changed, it is thus achieved that Jenner's popped rice nanoparticle.
Embodiment 4:
<1>preparation of golden nanometer particle seed
95mL high purity water and 400 μ L1.5wt% chlorauric acid solutions are added, as more than 90 DEG C in 250mL three-neck flask In water-bath, adding 6mL0.8wt% sodium citrate solution after 15~20min, the color of solution is reddened gradually by colourless, and Carrying out synthetic reaction water-bath 80 DEG C, after 13min, reaction terminates;Gained redness golden nanometer particle seed is placed in 100mL close Close in glass container, use in case next step prepares Jenner's popped rice nanoparticle;
<2>preparation of Jenner's popped rice nanoparticle
In the reaction bulb of 20mL, add 11mL high purity water, add the golden nanometer particle seed 250 μ L made in the first step, Magnetic agitation 15~to add 1500 μ L concentration after 20 minutes be 2000 μ g/L ethanolamine under 25 DEG C of water-baths;By dropping 1mol/L sodium hydroxide solution regulation pH is 10, proceeds to magnetic agitation in 50 DEG C of water-baths after 13min, reacts 75min, molten The color of liquid is from light red purpling, blue through purplish blue complexion changed, it is thus achieved that Jenner's popped rice nanoparticle.
Embodiment 5:
<1>preparation of golden nanometer particle seed
85mL high purity water and 350 μ L1.2wt% chlorauric acid solutions are added, as more than 90 DEG C in 250mL three-neck flask In water-bath, adding 5mL0.9wt% sodium citrate solution after 15~20min, the color of solution is reddened gradually by colourless, and Carrying out synthetic reaction water-bath 85 DEG C, after 14min, reaction terminates;Gained redness golden nanometer particle seed is placed in 100mL close Close in glass container, use in case next step prepares Jenner's popped rice nanoparticle;
<2>preparation of Jenner's popped rice nanoparticle
In the reaction bulb of 20mL, add 12mL high purity water, add the golden nanometer particle seed 300 μ L made in the first step, Magnetic agitation 15~to add 1800 μ L concentration after 20 minutes be 1800 μ g/L ethanolamine under 25 DEG C of water-baths;By dropping 1mol/L sodium hydroxide solution regulation pH is 11, proceeds to magnetic agitation in 55 DEG C of water-baths after 12min, reacts 65min, molten The color of liquid is from light red purpling, blue through purplish blue complexion changed, it is thus achieved that Jenner's popped rice nanoparticle.
As it is shown in figure 1, A-F represents the Jenner's popped rice nanoparticle ultraviolet scanning spectrum figure obtained by embodiment 1-5 respectively, can To find out that it has good concordance, there is near 650nm best assimilation effect;As in figure 2 it is shown, it is gold nano Flower nanoparticle ultraviolet Electronic Speculum figure, it can be clearly seen that the flower-like structure that this nanoparticle surface is coarse, specifically has star topology, Each nanoparticle averagely has 6-10 star branch.

Claims (7)

1. Jenner's popped rice nanoparticle, it is characterised in that the surface of this nanoparticle is flower-like structure.
2. the preparation method of the Jenner's popped rice nanoparticle described in claim 1, it is characterised in that comprise the following steps:
(1) preparation of golden nanometer particle seed:
First chlorauric acid solution added high purity water and carry out heating in water bath, adding sodium citrate solution, the color of solution by colourless gradually Gradual change is red, i.e. obtains red golden nanometer particle seed;
(2) preparation of Jenner's popped rice nanoparticle:
Take above-mentioned prepared golden nanometer particle seed and add high purity water, adding ethanolamine under water bath condition after magnetic agitation, regulate pH, Continuing water-bath magnetic agitation, solution colour is by light red purpling more blue through purplish blue complexion changed, finally gives Jenner's popped rice nanoparticle Finished product.
3. the preparation method of Jenner's popped rice nanoparticle as claimed in claim 2, it is characterised in that above-mentioned steps (1) concrete Operation is: adds 80-100ml high purity water and 200-500 μ l chlorauric acid solution in reaction vessel, is placed in more than 90 DEG C water In bath, adding sodium citrate solution, and carry out synthetic reaction water-bath 60~90 DEG C after 15-20min, the color of solution is by nothing Color reddens gradually, terminates after 8-15 minute;Gained red nano gold seeds is placed in closed glass container, in case next step system Standby Jenner's popped rice nanoparticle.
4. the preparation method of Jenner's popped rice nanoparticle as claimed in claim 2, it is characterised in that above-mentioned steps (2) concrete Operation is: add golden nanometer particle seed in high purity water and step (1), magnetic agitation under 15-30 DEG C of water-bath in reaction bulb Ethanolamine is added after 15-20 minute;By dropping sodium hydroxide solution regulation pH;40-70 DEG C of water-bath is proceeded to after 10-20 minute Middle magnetic agitation;After reaction 50-90min, the color of solution is from light red purpling, blue through purplish blue complexion changed, finally gives gold nano Flower nanoparticle finished product.
5. the preparation method of Jenner's popped rice nanoparticle as claimed in claim 3, it is characterised in that in above-mentioned steps (1): institute The concentration stating gold chloride is 0.5-2wt%;The concentration of described sodium citrate is 0.5-1wt%.
6. the preparation method of Jenner's popped rice nanoparticle as claimed in claim 4, it is characterised in that add in above-mentioned steps (2) Ethanolamine concentration is: 1000-2400 μ g/L, and volume is 500-2000 μ l;Golden nanometer particle seed volume: 100-300 μ l; Naoh concentration is 0.5-1.0mol/L;High purity water volume is 8-12mL;Regulation pH is 6-12.
7. the arbitrary described Jenner's popped rice nanoparticle of claim 1-6 is at development biological sensor, nanometer sensor, catalyst nano Application in element or nano electrochemical field.
CN201610251906.XA 2016-04-21 2016-04-21 Gold nanoflower nano-particle and preparation method thereof Pending CN105903948A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN106475574A (en) * 2016-11-30 2017-03-08 燕山大学 A kind of method preparing Jenner's popped rice
CN106568829A (en) * 2016-11-09 2017-04-19 信阳师范学院 Flower-like gold-silver nano compound electrochemical sensor, and preparation method and applications thereof
CN108254421A (en) * 2017-12-11 2018-07-06 东莞理工学院 Flower shape Au micro nano structures, modified electrode and preparation method and application
CN108693162A (en) * 2018-05-21 2018-10-23 浙江理工大学 A kind of Au@mSiO2Nano flower SERS substrates and preparation method thereof
CN108723386A (en) * 2018-06-11 2018-11-02 浙江大学 A kind of preparation method of the gold nano dendrite particle with photo-thermal effect
CN109192385A (en) * 2018-08-30 2019-01-11 广州创链科技有限公司 A kind of sweeping robot shielding drainage electric wire
CN110026568A (en) * 2019-04-25 2019-07-19 山东省医学科学院药物研究所(山东省抗衰老研究中心、山东省新技术制药研究所) A kind of method that polyhydroxy natural products mediates synthesis to carry medicinal dendritic nanogold particle
WO2023224898A1 (en) * 2022-05-17 2023-11-23 The Government Of The United States Of America, As Represented By The Secretary Of The Navy Seedless synthesis of anisotropic gold nanoflowers for cellular control and drug delivery applications

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106568829A (en) * 2016-11-09 2017-04-19 信阳师范学院 Flower-like gold-silver nano compound electrochemical sensor, and preparation method and applications thereof
CN106475574A (en) * 2016-11-30 2017-03-08 燕山大学 A kind of method preparing Jenner's popped rice
CN106475574B (en) * 2016-11-30 2018-06-08 燕山大学 A kind of method for preparing Jenner's popped rice
CN108254421A (en) * 2017-12-11 2018-07-06 东莞理工学院 Flower shape Au micro nano structures, modified electrode and preparation method and application
CN108254421B (en) * 2017-12-11 2019-09-27 东莞理工学院 Flower shape Au micro nano structure, modified electrode and preparation method and application
CN108693162A (en) * 2018-05-21 2018-10-23 浙江理工大学 A kind of Au@mSiO2Nano flower SERS substrates and preparation method thereof
CN108723386A (en) * 2018-06-11 2018-11-02 浙江大学 A kind of preparation method of the gold nano dendrite particle with photo-thermal effect
CN109192385A (en) * 2018-08-30 2019-01-11 广州创链科技有限公司 A kind of sweeping robot shielding drainage electric wire
CN110026568A (en) * 2019-04-25 2019-07-19 山东省医学科学院药物研究所(山东省抗衰老研究中心、山东省新技术制药研究所) A kind of method that polyhydroxy natural products mediates synthesis to carry medicinal dendritic nanogold particle
CN110026568B (en) * 2019-04-25 2021-12-24 山东省医学科学院药物研究所(山东省抗衰老研究中心、山东省新技术制药研究所) Method for synthesizing medicinal dendritic nano gold particles by mediation of polyhydroxy natural products
WO2023224898A1 (en) * 2022-05-17 2023-11-23 The Government Of The United States Of America, As Represented By The Secretary Of The Navy Seedless synthesis of anisotropic gold nanoflowers for cellular control and drug delivery applications

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