CN101230208A - Method for preparing gold nano-rod particles coated with silica layer - Google Patents
Method for preparing gold nano-rod particles coated with silica layer Download PDFInfo
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- CN101230208A CN101230208A CNA2008100556873A CN200810055687A CN101230208A CN 101230208 A CN101230208 A CN 101230208A CN A2008100556873 A CNA2008100556873 A CN A2008100556873A CN 200810055687 A CN200810055687 A CN 200810055687A CN 101230208 A CN101230208 A CN 101230208A
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Abstract
The invention discloses a method for preparing golden nanorod particles coated with silicon dioxide layers on the surfaces. The method adopts the steps that ammonia water is charged into a golden nanoparticle solution with stable CTAB to form a golden nanorod solution, and the golden nanorod solution is mixed with an ethyl alcohol solution of tetraethylorthosilicate for reaction, to obtain the golden nanoparticles coated with the silicon dioxide layers on the surfaces. In the invention, even silicon dioxide layers can be prepared on the surfaces of the golden nanorods with stable CTAB without the assistance of a polymer or a polyelectrolyte, and the thickness of the silicon dioxide layers can be controlled by changing the quantity of TEOS, therefore, the invention has the advantages of simple operation and temperate condition, and has universal guiding significances for the preparation of the anisotropic nano material coated with the silicon dioxide layers.
Description
Technical field
The present invention relates to the method that a kind of preparation is coated with the gold nano-rod particles of silicon dioxide layer.
Background technology
In recent years, people have been developed the number of chemical method, metal nanoparticle [the J.P é rez-Juste for preparing each diversity, et al.Coord.Chem.Rev.2005,249,1870], wherein successful is to utilize cats product cetyl trimethyl ammonia bromide (CTAB) to induce reagent to come controlling dimension and shape as pattern.Up to the present, utilize CTAB solution controlling dimension and pattern, research is clear that the synthetic of gold nanorods the most.People can realize the fine adjustments of gold nanorods optical property, by the major-minor axis ratio of control gold nanorods, realize the fine adjustments [B.Nikoobakht of its optical property from the visible region to the near-infrared region, M.A.El-Sayed, Chem.Mater.2003,15,1957; J.P é rez-Juste, et al.Adv.Funct.Mater.2005,15,1065].Because the special optical characteristic of gold nanorods makes gold nanorods be with a wide range of applications in fields such as biosensor, bio-imaging, biomarkers.Though yet CTAB micella environment helps the stability of gold nano-rod particles, but the existence of CTAB molecule brings a series of problem: (1) CTAB molecule is at the stable existence on gold nanorods surface, hydrophobization that make the to realize gold nanorods surface difficulty [Nikoobakht that becomes, B.El-Sayed, M.A.Langmuir 2001,17,6368.].Have only several pieces of articles to report recently and successfully handle this problem, realize that the stable gold nanorods of CTAB disperses in organic solvent, but this is [Yang, J.Wu, the J.et al.Chem.Phys.Lett.2005 that realizes under very harsh experiment condition, 416,215.Wei, G.-T.Yang, Z.et al.J.Am.Chem.Soc.2004,126,5036.].(2) the CTAB molecule is in the existence on gold nanorods surface, makes the bio-modification on the gold nanorods surface difficulty that becomes, and the CTAB molecule has bio-toxicity, seriously like this limited the application of gold nano-rod particles at biological field.Because silicon-dioxide has the modifiability on outstanding chemical stability, biocompatibility, surface, make at the stable gold nanorods surface parcel silicon dioxide layer of CTAB, become one of the in-problem optimal selection scheme in the stable gold nano-rod particles biologic applications of CTAB that solves.
People have reported at the surface of the gold nano grain of citrate-stable parcel silicon-dioxide, mainly contain following two main patterns: (1) utilizes silanization coupling reagent (aminopropyl organoalkoxysilane (APTMS) or sulfydryl propyl group organoalkoxysilane (MPTMS)) [Liz-Marza ' n, L.M.Giersig, M.Mulvaney, P.Langmuir 1996,12,4329.], (2) use polyvinylpyrrolidone (PVP) to handle nano material, hydrolysis tetraethoxy (TEOS) prepares silicon dioxide layer [Graf, C.Vossen, D.L.J.et al.Langmuir2003 in the ammonia soln of ethanol or Virahol then, 19,6693.].The use of this two classes reagent not only can promote nano material to transfer in the alcohol, and can promote the formation of silicon dioxide layer.Yet,,, make and utilize APTMS or MPTMS to replace CTAB in become unusual difficulty of the surface adsorption of gold grain because the CTAB molecule is bonded in the surface of gold nanorods very securely for the stable gold nanorods of CTAB.Although people such as Murphy and Pastoriza-Santos is [Obare, S.O.Jana, N.R.Murphy, C.J.Nano Lett.2001,1,601.Pe ' rez-Juste, J.Correa-Duarte, M.A.et al.Appl.Surf.Sci.2004,226,137.] reported in succession and utilized MPTMS parcel gold nano grain, and utilize sodium metasilicate at the stable gold nanorods surface preparation silicon dioxide layer of CTAB, but the poor repeatability of their method, and in the process that adds sodium metasilicate, be easy to occur the phenomenon of particle aggregation.When using the stable gold nanorods of PVP parcel CTAB to prepare silicon dioxide layer in addition, the silicon dioxide layer that the gold nanorods surface forms is uneven.People such as Pastoriza-Santos [I.Pastoriza-Santos, J.Pe ' rez-Juste, et al.Chem.Mater.2006,18,2645.] have reported a kind of method, can realize the even coating of silicon-dioxide on the gold nano-rod particles surface.In their method, the layer-by-layer of polyelectrolyte is combined with tetraethoxy (TEOS) controlled hydrolysis in the isopropanol water solution, go out evenly and the silicon dioxide layer of controllable thickness in the gold nanorods surface preparation.After the unnecessary Surfactant CTAB of their at first centrifugal removal, gold nano-rod particles is scattered in the water, under intense stirring condition, dropwise adds electronegative polyelectrolyte, repeat then to handle with the polyelectrolyte of positively charged, eccentric cleaning is removed unnecessary polyelectrolyte then.Two kinds of polyelectrolyte layers can thoroughly shield or cover the CTAB effect on gold nanorods surface.The gold nano-rod particles that to handle is transferred to hydrolysis TEOS in the solution of Virahol and ammoniacal liquor then, the preparation silicon dioxide layer.
But in this method, there is following problem: (1) complicated operation.Preparation process has been used PVP and has been used the polyelectrolyte of positively charged and electronegative polyelectrolyte to handle repeatedly, and repeatedly after the centrifugal treating, transfers in the Virahol, carries out the hydrolysis of TEOS again, the preparation silicon dioxide layer.(2) condition control requires harsh.The molecular weight of employed PVP of preparation process and polyelectrolyte and the ionic strength of reaction will have strict restriction, because high molecular weight polymers can produce bridge linking effect, and then the gathering between the generation particle, high ionic strength causes producing the gathering between the particle equally easily.
Summary of the invention
The purpose of this invention is to provide the method that a kind of preparation is coated with the gold nano-rod particles of silicon dioxide layer.
The present invention's preparation is coated with the method for the gold nano-rod particles of silicon dioxide layer, be in the stable gold nano-rod particles solution of CTAB, to add ammoniacal liquor to form gold nanorods solution, with the mixed reaction of the ethanolic soln of described gold nanorods solution and tetraethoxy, obtain the described gold nano-rod particles that is coated with silicon dioxide layer then.
Wherein, the pH of gold nanorods solution is 6-12.Preferably, be that described gold nano-rod particles solution is joined in the ethanolic soln of described tetraethoxy with the mixed reaction of the ethanolic soln of described gold nano-rod particles solution and tetraethoxy.
In the preparation process, gold nanorods and tetraethoxy consumption mole ratio are 100: 1～1: 200 relation.Preferably, the mole ratio of gold nanorods and tetraethoxy is 10: 1～1: 50.The concentration of the ethanolic soln of described tetraethoxy is 0.1mmol/L-2mol/L.Reaction is more than 1 hour under the room temperature.
The present invention does not need to add the help of polymkeric substance or polyelectrolyte, just can go out uniform silicon dioxide layer in the stable gold nanorods surface preparation of CTAB, and by changing the amount of TEOS, can control the thickness of silicon dioxide layer.Therefore method provided by the invention has outstanding advantage easy and simple to handle, mild condition, and the even and thickness of silicon dioxide layer is controlled easily, and has general directive significance for the preparation of the nano material parcel silicon dioxide layer with each diversity.
Description of drawings
Fig. 1 is the transmission electron microscope photo behind the embodiment 1 gold nanorods parcel silicon-dioxide;
Fig. 2 is the transmission electron microscope photo behind the embodiment 2 gold nanorods parcel silicon-dioxide;
Fig. 3 is the transmission electron microscope photo behind the embodiment 3 gold nanorods parcel silicon-dioxide.
Embodiment
The present invention's preparation is coated with the method for the gold nano-rod particles of silicon dioxide layer, be in the stable gold nano-rod particles solution of cetyl trimethyl ammonia bromide (CTAB), to add ammoniacal liquor, then gold nano-rod particles solution is joined in the ethanolic soln of tetraethoxy (TEOS), make the TEOS hydrolysis, by the control alr mode, uniform silicon dioxide layer is directly prepared on the surface that just can be implemented in the stable gold nano of CTAB.
In above-mentioned preparation process, add ammoniacal liquor and make that the pH of gold nano-rod particles solution is 6-14, the concentration of the ethanolic soln of tetraethoxy (TEOS) is 0.1mmol/L-2mol/L, the consumption mole ratio of gold nano-rod particles and TEOS is 100: 1～1: 200.Entire reaction is carried out more than 1 hour at 5-80 ℃.
The present invention does not need to add the help of polymkeric substance or polyelectrolyte, just can be at the stable uniform silicon dioxide layer of gold nanorods surface preparation of CTAB, and, can control the thickness of silicon dioxide layer by changing the amount of TEOS, the thickness of gained silicon dioxide layer generally can be controlled in 1-500nm.
The base program of the gold nano grain of concrete preparation coated with silica:
(1) the stable gold nano-rod particles of reference literature [J.Phys.Chem.B 2005,109,13857.] preparation CTAB.
(2) preparation (Au of the gold nano grain of coated with silica
Rod@SiO
2): the gold nano-rod particles centrifugal treating with step (1) preparation is dispersed in throw out in the ultrapure water.Utilize ammoniacal liquor to regulate gold nano-rod particles pH value of solution value～10 then.The ethanolic soln that adds tetraethoxy (TEOS) subsequently stirs (magnetic agitation, mechanical stirring, vibration stirring etc.), allows solution continue reaction.Centrifugal collection Au after reaction is finished
Rod@SiO
2, water and ethanol clean respectively then, obtain the gold nano grain of coated with silica.By the amount of the different TEOS of control adding, can regulate and control SiO
2The thickness of shell.
Embodiment 1:
(1) reference literature [J.Phys.Chem.B 2005,109,13857] preparation gold nano-rod particles;
(2) preparation (Au of the gold nano grain of coated with silica
Rod@SiO
2): the gold nano-rod particles solution 20mL centrifugal treating with step (1) preparation is dispersed in throw out in the ultrapure water.Utilize ammoniacal liquor to regulate pH value～10 of gold nano-rod particles solution then.Adding concentration subsequently is the TEOS ethanolic soln 4mL of 1mmol/L, adopts the mechanical stirring mode, allows solution continue reaction.Centrifugal collection Au after reaction is finished
Rod@SiO
2, water and ethanol clean respectively then.Be the Au of shell at last with silicon-dioxide
Rod@SiO
2Nanoparticle is dispersed in the ethanol, obtains the gold nano-rod particles that thickness is approximately the silicon dioxide layer coating of 6nm.Transmission electron microscope photo such as Fig. 1 behind the gold nanorods parcel silicon-dioxide, illustration wherein is the part enlarged view.From figure, can clearly be seen that and be wrapped with silicon dioxide layer at gold nanorods.
Embodiment 2:
(1) reference literature [J.Phys.Chem.B 2005,109,13857] preparation gold nano-rod particles;
(2) preparation (Au of the gold nano grain of coated with silica
Rod@SiO
2): the gold nano-rod particles solution 20mL centrifugal treating with step (1) preparation is dispersed in throw out in the ultrapure water.Utilize ammoniacal liquor to regulate pH value～10 of gold nano-rod particles solution then.Adding concentration subsequently is the TEOS ethanolic soln 8mL of 1mmol/L, adopts the magnetic agitation mode, allows solution continue reaction.Centrifugal collection Au after reaction is finished
Rod@SiO
2, water and ethanol clean respectively then.Obtain the gold nano-rod particles that thickness is approximately the coated with silica of 16nm at last, its transmission electron microscope photo such as Fig. 2.From figure, can clearly be seen that and be wrapped with silicon dioxide layer at gold nanorods.
Embodiment 3:
(1) reference literature [J.Phys.Chem.B 2005,109,13857] preparation gold nano-rod particles;
(2) preparation (Au of the gold nano grain of coated with silica
Rod@SiO
2): the gold nano-rod particles solution 20mL centrifugal treating with step (1) preparation is dispersed in throw out in the ultrapure water.Utilize ammoniacal liquor to regulate pH value～10 of gold nano-rod particles solution then.Adding concentration subsequently is the TEOS ethanolic soln 16mL of 1mmol/L, adopts the vibration alr mode, allows solution continue reaction.Centrifugal collection Au after reaction is finished
Rod@SiO
2, water and ethanol clean respectively then.Obtain the gold nano-rod particles that thickness is approximately the coated with silica of 25nm at last, its transmission electron microscope photo such as Fig. 3.From figure, can clearly be seen that and be wrapped with silicon dioxide layer at gold nanorods.
Claims (7)
1. method for preparing the gold nano-rod particles that is coated with silicon dioxide layer, be in the stable gold nano-rod particles solution of CTAB, to add ammoniacal liquor to form gold nanorods solution, with the mixed reaction of the ethanolic soln of described gold nanorods solution and tetraethoxy, obtain the described gold nano-rod particles that is coated with silicon dioxide layer then.
2. method according to claim 1 is characterized in that: the pH of described gold nanorods solution is 6-14.
3. method according to claim 1 is characterized in that: with the mixed reaction of the ethanolic soln of described gold nanorods solution and tetraethoxy is that described gold nanorods solution is joined in the ethanolic soln of described tetraethoxy.
4. method according to claim 1 is characterized in that: the concentration of the ethanolic soln of described tetraethoxy is 0.1mmol/L to 2mol/L.
5. method according to claim 4 is characterized in that: the gold nanorods in the described gold nanorods solution and the mole ratio of tetraethoxy consumption are 100: 1～1: 200.
6. method according to claim 5 is characterized in that: the mole ratio of gold nanorods and tetraethoxy is 10: 1～1: 50.
7. according to the arbitrary described method of claim 1-6, it is characterized in that: temperature of reaction is 5-80 ℃, and the reaction times is no less than 1 hour.
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| CN101608181B (en) * | 2009-06-01 | 2010-12-08 | 首都师范大学 | Preparation method of gold nanorod/glucose oxidase composite particles |
| CN101982774A (en) * | 2010-09-30 | 2011-03-02 | 暨南大学 | Biological functionalized gold nanorod molecular probe as well as preparation method and application thereof |
| CN102078617A (en) * | 2010-12-28 | 2011-06-01 | 中国科学院上海硅酸盐研究所 | Method for synthesizing mesoporous silica-based nanocomposite embedded with gold nanorods |
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| CN101608181B (en) * | 2009-06-01 | 2010-12-08 | 首都师范大学 | Preparation method of gold nanorod/glucose oxidase composite particles |
| CN101982774A (en) * | 2010-09-30 | 2011-03-02 | 暨南大学 | Biological functionalized gold nanorod molecular probe as well as preparation method and application thereof |
| CN101982774B (en) * | 2010-09-30 | 2013-07-24 | 暨南大学 | Biological functionalized gold nanorod molecular probe as well as preparation method and application thereof |
| CN102091344A (en) * | 2010-11-17 | 2011-06-15 | 无锡中科光远生物材料有限公司 | Gold nanorod-chitosan film and preparation method thereof |
| CN102078617A (en) * | 2010-12-28 | 2011-06-01 | 中国科学院上海硅酸盐研究所 | Method for synthesizing mesoporous silica-based nanocomposite embedded with gold nanorods |
| CN102078617B (en) * | 2010-12-28 | 2012-05-30 | 中国科学院上海硅酸盐研究所 | Method for synthesizing mesoporous silica-based nanocomposite embedded with gold nanorods |
| CN102756125B (en) * | 2011-04-25 | 2015-04-08 | 韩国科学技术研究院 | Method for fabricating nanohybrids, the nanohybrids |
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