CN103198913B - Silver-tri-iron tetroxide core shell nanoparticles and preparation method thereof - Google Patents
Silver-tri-iron tetroxide core shell nanoparticles and preparation method thereof Download PDFInfo
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- CN103198913B CN103198913B CN201210014091.5A CN201210014091A CN103198913B CN 103198913 B CN103198913 B CN 103198913B CN 201210014091 A CN201210014091 A CN 201210014091A CN 103198913 B CN103198913 B CN 103198913B
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Abstract
The invention discloses a kind of silver-tri-iron tetroxide core shell nanoparticles and preparation method thereof.The Core-shell Structure Nanoparticles that particle is is core with silver, tri-iron tetroxide is shell, its particle diameter is 160 ~ 230nm, wherein, silver for particle diameter be the silver nano-grain of 60 ~ 90nm, the shell of tri-iron tetroxide shell is thick is 50 ~ 70nm; Method is be first the ratio of 1: 0.15 ~ 0.6: 0.175 ~ 0.225 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate are dissolved in ethylene glycol, and stir at least 25min, obtain mixed liquor, again sodium acetate is added in mixed liquor, wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 0.8 ~ 1.2: 9, obtain front body liquid, subsequently, front body liquid is placed in air-tight state, at 180 ~ 220 DEG C, reacts 4 ~ 24h, obtained silver-tri-iron tetroxide core shell nanoparticles.Its optical property is extensively adjustable in ultraviolet-visible near infrared region, and has fabulous magnetic responsiveness, will be with a wide range of applications and huge potentiality in biomedicine.
Description
Technical field
The present invention relates to a kind of core shell nanoparticles and preparation method, especially a kind of silver-tri-iron tetroxide nucleocapsid (AgFe
3o
4) nano particle and preparation method thereof.
Background technology
Along with the develop rapidly of the subjects such as nanometer technology and material science, physical chemistry, biomedical technology, the material with single performance can not meet the demand of practical application far away, therefore designs and controls synthesis to have the polyfunctional nano material of special construction extremely urgent.By the function and service of two or more materials, performance complement and optimization, the hybrid material of excellent performance can be prepared.The character of hybrid material be not only simply adding of each constitutive property and, and their active forces that both can also be utilized mutual, form that structure is homogeneous, the new material of excellent performance; The physics that same compound shows or chemical property can be interrelated or have cooperative effect.Core-shell type nano material is owing to having gathered the premium properties of core, shell component, by to nucleocapsid structure, the cutting out of size, the character such as magnetics, optics, mechanics, calorifics, electricity, catalysis of controllable composite material, the compound designed, synthesis has the multiple physical propertys such as optical, electrical, magnetic is simultaneously made to become possibility, this novel material has the advantage of multiple performance simultaneously, has become one of heat subject of the research field such as material science and information science; As " a kind of preparation method of silver/magnetic nanometer particle " that describe in the Chinese invention patent specification CN100460338C that announces on February 11st, 2009.The particle diameter of the silver/magnetic nanometer particle mentioned in this specification is 60 ± 20nm, and its kernel is tri-iron tetroxide, shell is elemental silver; Preparation method is in the aqueous phase of Reverse Microemulsion System, liquor argenti nitratis ophthalmicus with magnetic ferroferric oxide nanometer particle for kernel, by reduction reaction, elemental silver is deposited on the surface of ferroferric oxide nano granules, thus obtains the end product with coreshell type structure.But, no matter be silver/magnetic nanometer particle, or its preparation method, all there is shortcoming part, first, though end product has good fungistatic effect, do not possess the adjustability of optical property, be difficult to use in various fields optical property adjustability being had to requirement; Secondly, after elemental silver coated ferriferrous oxide, the normal performance of Fe 3 O 4 magnetic energy can be had influence on, magnetic responsiveness is deteriorated; Finally, preparation method can not obtain other target product except end product, to overcome the above-mentioned defect of end product.
Summary of the invention
The technical problem to be solved in the present invention, for overcoming shortcoming part of the prior art, provides a kind of rational in infrastructure, silver-tri-iron tetroxide core shell nanoparticles that optical absorption characteristics is adjustable in visible-near-infrared district.
Another technical problem that the present invention will solve is for providing a kind of preparation method of above-mentioned silver-tri-iron tetroxide core shell nanoparticles.
For solving technical problem of the present invention, the technical scheme adopted is: silver-tri-iron tetroxide core shell nanoparticles comprises silver, particularly,
Described silver is coated with tri-iron tetroxide, and described take silver as core, tri-iron tetroxide is shell nucleocapsid structure is graininess, and the particle diameter of described particle is 160 ~ 230nm;
Described silver is silver nano-grain, and the particle diameter of described silver nano-grain is 60 ~ 90nm;
The shell of described tri-iron tetroxide shell is thick is 50 ~ 70nm.
As the further improvement of silver-tri-iron tetroxide core shell nanoparticles, the ferroferric oxide nano granules that described tri-iron tetroxide shell is 5 ~ 20nm by particle diameter is formed.
For solving another technical problem of the present invention, another technical scheme adopted is: the preparation method of above-mentioned silver-tri-iron tetroxide core shell nanoparticles adopts hydro thermal method, and particularly completing steps is as follows:
Step 1, be first the ratio of 1: 0.15 ~ 0.6: 0.175 ~ 0.225 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate are dissolved in ethylene glycol, and stir at least 25min, obtain mixed liquor, then sodium acetate is added in mixed liquor, wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 0.8 ~ 1.2: 9, obtains front body liquid;
Step 2, is placed in air-tight state by front body liquid, at 180 ~ 220 DEG C, react 4 ~ 24h, and obtained sediment, described sediment is silver-tri-iron tetroxide core shell nanoparticles.
As the further improvement of the preparation method of silver-tri-iron tetroxide core shell nanoparticles, described ferric nitrate and silver nitrate are dissolved in ethylene glycol after, the time of stirring is 25 ~ 35min; Described sediment to be washed, be separated and the process of drying; Described carrying out washing treatment replaces cleaning 5 ~ 7 times for using ethanol and deionized water; Described separating treatment is separated for using magnet; Described drying is treated to dry 3h at 70 DEG C.
Relative to the beneficial effect of prior art be, one, ESEM, transmission electron microscope and its subsidiary power spectrum test component are used respectively to obtained target product, and X-ray diffractometer characterizes, from its result, target product is the nano particle of numerous good nucleocapsid structures of dispersiveness of uniform size, and its particle diameter is 160 ~ 230nm, and the shell that the particle being 60 ~ 90nm by particle diameter is core, its granular substance being coated with thick 50 ~ 70nm forms is formed; Wherein, power spectrum test component demonstrates its centre to the Surface scan of single core core-shell nanoparticles and line sweep result and is dispersed with silver element, and iron, oxygen element are distributed in various piece, the core demonstrating core shell nanoparticles is iron oxide for silver, shell, namely confirm target product be core with silver, the tri-iron tetroxide nucleocapsid structure that is shell.They are two years old, ultraviolet-visible-near infrared spectrometer and superconducting quantum interference device (SQUID) is used to characterize respectively to obtained target product, from its result, along with the change of the particle diameter of target product kernel and the thickness of shell, its optical property all there occurs and changes significantly in ultraviolet-visible near infrared region.Meanwhile, target product also presents superparamagnetism, and its saturation magnetization is at least 50emu/g, and remanent magnetization and coercive force are zero.They are three years old, preparation method's science, effectively, both the core shell nanoparticles that to have prepared take silver as core, tri-iron tetroxide is shell, make again the optical property of the target product obtained extensively adjustable in ultraviolet-visible near infrared region, and there is fabulous magnetic responsiveness, make it will be with a wide range of applications in biomedicine and huge potentiality, also have raw material few, simple process, is suitable for the feature of industrializing implementation.
As the further embodiment of beneficial effect, one is that the ferroferric oxide nano granules that tri-iron tetroxide shell is preferably 5 ~ 20nm by particle diameter is formed, and is beneficial to the specific area increasing target product, expands its range of application and field.Two is that after ferric nitrate and silver nitrate are dissolved in ethylene glycol, the time of stirring is preferably 25 ~ 35min, can obtain the mixed liquor stirred.Three is preferably wash sediment, be separated and the process of drying, wherein, carrying out washing treatment is preferably and uses ethanol and deionized water to replace cleaning 5 ~ 7 times, separating treatment is preferably and uses magnet to be separated, dry process is preferably dry 3h at 70 DEG C, ensure that degree of purity and the quality of target product.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, optimal way of the present invention is described in further detail.
Fig. 1 is to one of result that obtained target product uses ESEM (SEM) and transmission electron microscope (TEM) to characterize respectively.
Fig. 2 is to one of result that target product uses X-ray diffraction (XRD) instrument to characterize.
Fig. 3 is to one of result that obtained different size target product uses ultraviolet-visible-near infrared spectrometer to characterize with the target product using different mol ratio value presoma to obtain.
Fig. 4 is to one of result that obtained target product uses superconductive quantum interference (SQUID) instrument to characterize.
Embodiment
First buy from market or obtain by conventional method:
Ferric nitrate; Silver nitrate; Ethylene glycol; Sodium acetate.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1, is first the ratio of 1: 0.15: 0.225 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate is dissolved in ethylene glycol, and stirs 25min, obtain mixed liquor.Again sodium acetate is added in mixed liquor; Wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 0.8: 9, obtains front body liquid.
Step 2, is placed in air-tight state by front body liquid, at 180 DEG C, reacts 24h; Obtain and be similar to shown in Fig. 1, and the sediment as shown in the curve in Fig. 2, Fig. 3 and Fig. 4---silver-tri-iron tetroxide core shell nanoparticles.
Embodiment 2
The concrete steps of preparation are:
Step 1, is first the ratio of 1: 0.26: 0.213 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate is dissolved in ethylene glycol, and stirs 28min, obtain mixed liquor.Again sodium acetate is added in mixed liquor; Wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 0.9: 9, obtains front body liquid.
Step 2, is placed in air-tight state by front body liquid, at 190 DEG C, reacts 19h; Obtain and be similar to shown in Fig. 1, and the sediment as shown in the curve in Fig. 2, Fig. 3 and Fig. 4---silver-tri-iron tetroxide core shell nanoparticles.
Embodiment 3
The concrete steps of preparation are:
Step 1, is first the ratio of 1: 0.38: 0.2 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate is dissolved in ethylene glycol, and stirs 30min, obtain mixed liquor.Again sodium acetate is added in mixed liquor; Wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 1: 9, obtains front body liquid.
Step 2, is placed in air-tight state by front body liquid, at 200 DEG C, reacts 14h; Obtain as shown in Figure 1, and the sediment as shown in the curve in Fig. 2, Fig. 3 and Fig. 4---silver-tri-iron tetroxide core shell nanoparticles.
Embodiment 4
The concrete steps of preparation are:
Step 1, is first the ratio of 1: 0.49: 0.188 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate is dissolved in ethylene glycol, and stirs 33min, obtain mixed liquor.Again sodium acetate is added in mixed liquor; Wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 1.1: 9, obtains front body liquid.
Step 2, is placed in air-tight state by front body liquid, at 210 DEG C, reacts 8h; Obtain and be similar to shown in Fig. 1, and the sediment as shown in the curve in Fig. 2, Fig. 3 and Fig. 4---silver-tri-iron tetroxide core shell nanoparticles.
Embodiment 5
The concrete steps of preparation are:
Step 1, is first the ratio of 1: 0.6: 0.175 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate is dissolved in ethylene glycol, and stirs 35min, obtain mixed liquor.Again sodium acetate is added in mixed liquor; Wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 1.2: 9, obtains front body liquid.
Step 2, is placed in air-tight state by front body liquid, at 220 DEG C, reacts 4h; Obtain and be similar to shown in Fig. 1, and the sediment as shown in the curve in Fig. 2, Fig. 3 and Fig. 4---silver-tri-iron tetroxide core shell nanoparticles.
By the result characterized---Fig. 1 ~ Fig. 4 confirms that target product is silver-tri-iron tetroxide core shell nanoparticles: wherein,
Fig. 1 a of Fig. 1 is the SEM image of target product, and the illustration in its upper right corner is powerful SEM image, can be found out by it, and target product is graininess, and its surface is made up of many tiny nano particles; Fig. 1 b is the TEM image of target product, and the center and the outer rim that show target product also exist obvious contrast difference, confirm that target product is nucleocapsid structure.In conjunction with the subsidiary power spectrum test component of transmission electron microscope to the Surface scan of single target product and line sweep result, the nucleocapsid structure that known target product is is core with silver, tri-iron tetroxide is shell.
Have two cover Bragg diffraction peaks to occur in the XRD spectra of Fig. 2, wherein, 30.3 degree, 35.5 degree, 43.1 degree, 53.5 degree, 57.1 degree and 62.5 degree is Fe
3o
4(220), (311), (400), (422), (511) and (440) diffraction maximum; 38.1 degree, 44.3 degree, 64.4 degree and 77.3 degree then correspond to the diffraction maximum of (111), (200), (220) and (311) of Ag.
Fig. 3 a of Fig. 3 is the light absorption spectrogram of different size target product, curve 1 in spectrogram, curve 2 and curve 3 are respectively when hydrothermal conditions is respectively 4h, 8h and 24h, the diameter of corresponding galactic nucleus is respectively 60nm, 70nm and 90nm, and the thickness of tri-iron tetroxide shell is respectively light absorption line when 55nm, 65nm and 70nm, by the curve 1 of Fig. 3 a, curve 2 and curve 3 can be found out, along with the prolongation in reaction time, tri-iron tetroxide thickness from 55nm to 65nm and and then be increased to 70nm, the dipole resonance peak of target product there occurs obvious red shift, namely from the red shift of 390nm difference to 712nm, 764nm and 789nm, this causes the dielectric refractive index in metal surface is very responsive due to surface plasma body resonant vibration, based on tri-iron tetroxide dielectric constant (2.42) much larger than silver (0.399), thus cause the red shift at the plasmon absorption peak of silver particles, the movement of this metallic plasma resonance absorbing peak also meets Mie theory completely, simultaneously, target product be positioned at 392nm, the level Four formant of 424nm and 430nm has also occurred.Fig. 3 b is the light absorption spectrogram of the target product using different mol ratio value presoma to obtain, and the curve 1 in spectrogram, curve 2 and curve 3 mol ratio be respectively when the silver nitrate and ferric nitrate of preparing target product is respectively light absorption line when 0.15,0.30 and 0.60; Can be found out by the curve 1 of Fig. 3 b, curve 2 and curve 3, along with the increase of the mol ratio of silver nitrate and ferric nitrate, the dipole resonance absworption peak generation blue shift of silver particles, namely when the mol ratio of silver nitrate and ferric nitrate is 0.15, dipole resonance peak is positioned at 764nm, and when its ratio is increased to 0.30 and 0.6 respectively, dipole resonance peak difference blue shift is to 532nm and 500nm.
As seen from Figure 4, target product has fabulous superparamagnetism, and its saturation magnetization is 50 ~ 65emu/g, and remanent magnetization and coercive force are zero; This shows that granular target product has superparamagnetic performance, namely when without externally-applied magnetic field, it is without any magnetic, can not cause because magnetic attracts each other, agglomeration occurring between particle, and only when particle is in externally-applied magnetic field, just show the character of magnet, and with the increase of applied field strengths, its magnetic strengthens gradually, and this characteristic is highly advantageous to and uses external magnetic field carry out being separated to it and reclaim.
If obtain the target product of higher degree and quality, can wash the sediment obtained again, be separated and the process of drying; Wherein, carrying out washing treatment replaces cleaning 5 ~ 7 times for using ethanol and deionized water, and separating treatment is separated for using magnet, and drying is treated to dry 3h at 70 DEG C.
Obviously, those skilled in the art can carry out various change and modification to silver of the present invention-tri-iron tetroxide core shell nanoparticles and preparation method thereof and not depart from the spirit and scope of the present invention.Like this, if belong within the scope of the claims in the present invention and equivalent technologies thereof to these amendments of the present invention and modification, then the present invention is also intended to comprise these change and modification.
Claims (6)
1. a preparation method for silver-tri-iron tetroxide core shell nanoparticles, adopts hydro thermal method, it is characterized in that completing steps is as follows:
Step 1, be first the ratio of 1: 0.15 ~ 0.6: 0.175 ~ 0.225 according to ferric nitrate, mol ratio between silver nitrate and ethylene glycol, ferric nitrate and silver nitrate are dissolved in ethylene glycol, and stir at least 25min, obtain mixed liquor, then sodium acetate is added in mixed liquor, wherein, the mol ratio of the ferric nitrate in sodium acetate and mixed liquor is 0.8 ~ 1.2: 9, obtains front body liquid;
Step 2, is placed in air-tight state by front body liquid, at 180 ~ 220 DEG C, react 4 ~ 24h, obtained sediment, and described sediment is silver-tri-iron tetroxide core shell nanoparticles;
The particle diameter of described silver-tri-iron tetroxide core shell nanoparticles is 160 ~ 230nm, and its silver nano-grain being 60 ~ 90nm by particle diameter is core, the tri-iron tetroxide of the thick 50 ~ 70nm of being of shell is that shell forms.
2. the preparation method of silver according to claim 1-tri-iron tetroxide core shell nanoparticles, after it is characterized in that ferric nitrate and silver nitrate are dissolved in ethylene glycol, the time of stirring is 25 ~ 35min.
3. the preparation method of silver according to claim 1-tri-iron tetroxide core shell nanoparticles, is characterized in that washing sediment, is separated and the process of drying.
4. the preparation method of silver according to claim 3-tri-iron tetroxide core shell nanoparticles, is characterized in that carrying out washing treatment is use ethanol and deionized water to replace cleaning 5 ~ 7 times.
5. the preparation method of silver according to claim 3-tri-iron tetroxide core shell nanoparticles, is characterized in that separating treatment is use magnet to be separated.
6. the preparation method of silver according to claim 3-tri-iron tetroxide core shell nanoparticles, is characterized in that drying is treated to dry 3h at 70 DEG C.
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| CN104575677A (en) * | 2014-12-23 | 2015-04-29 | 合肥中南光电有限公司 | Electric conduction silver paste for filter |
| CN105842229B (en) * | 2016-06-15 | 2018-09-04 | 吉林大学 | A kind of nucleocapsid SERS probes, preparation method and its application in trace arsenic acid ion context of detection |
| CN108097950A (en) * | 2017-12-25 | 2018-06-01 | 浙江理工大学 | A kind of nucleocapsid Ag@Fe3O4Complex microsphere, preparation method and applications |
| CN109802127B (en) * | 2019-03-25 | 2021-08-13 | 东北大学 | Preparation method of silver-doped ferroferric oxide nano composite material |
| CN111691006B (en) * | 2020-07-29 | 2022-10-18 | 江苏惠康特种纤维有限公司 | Medical antibacterial ES fiber and preparation process thereof |
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