CN109971467A - A method of preparing gold nano particle modification fluorescence silicon nanorod - Google Patents
A method of preparing gold nano particle modification fluorescence silicon nanorod Download PDFInfo
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- CN109971467A CN109971467A CN201910240609.9A CN201910240609A CN109971467A CN 109971467 A CN109971467 A CN 109971467A CN 201910240609 A CN201910240609 A CN 201910240609A CN 109971467 A CN109971467 A CN 109971467A
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Abstract
The invention discloses a kind of methods for preparing gold nano particle modification fluorescence silicon nanorod, under the conditions of microwave radiation, gold ion is reduced into gold nano grain and growth in situ on fluorescence silicon nanorod surface, to synthesize a kind of new one-dimensional functionalized silicon nano material, it is with good water dispersible and preferable fluorescent stability, there is very strong absorption near infrared light, near infrared light thermal conversion efficiency with higher, photoacoustic signal can be generated to be imaged for real-time biological, be expected to be further used for bioanalysis detection field.
Description
Technical field
The invention belongs to technical field of nano material, are related to a kind of method for preparing silicon nano material, and in particular to a kind of
The method for preparing gold nano particle modification fluorescence silicon nanorod.
Background technique
As the important branch of nano material, silicon nano material is since (excellent biocompatibility enriches its plurality of advantages
Reserves, unique electricity, optics and mechanical property, and the compatibility with conventional silicon), in the energy, catalysis, photoelectron and life
The fields such as object are widely used.Especially in field of biomedicine (such as bio-sensing, inside and outside bio-imaging, cancer
Diagnoses and treatment etc.), the unique optics of function silicon nano material, magnetism and mechanical property are that the complexity that research tradition is difficult to capture is raw
Object process provides new opportunity and strategy, imply that biology and the infusive approach of field of biomedicine
(Nat.Mater.2009,8 (4), 331-336;Nano Lett.2012,12 (4), 1845-1850Science 2014,346,
1247390.).Therefore, in order to meet growing application demand, designing, there is the silicon of novel specific structure and functionalization to receive
Rice material becomes particularly significant.
In in the past few decades, researcher attempt a series of design of approach have specific structure (such as: silicon nanometer
Grain, silicon nanowires, silicon nanorod and silicon nanosphere) silicon nano material.One-dimensional silicon nanowires (SiNWs) has been developed as electrification
It learns and optical biosensor detects various biological targets in a manner of highly sensitive and specificity.Based on this, the silicon of functionalization
Nano wire is also that biological sensory field (such as: field effect transistor, Surface enhanced Raman scattering) provides new application platform, and
It can be achieved to include: nucleic acid, protein, metal ion and single celled highly sensitive detection (Science 2006,313,1100-
1104;Nat.Nanotechnol.2010,5,138;ACS Nano 2012,6,2582.).It is worth noting that, a kind of novel
One-dimensional fluorescence silicon nanostructure (J.Am.Chem.Soc.2016,138,4824), i.e. silicon nanorod (SiNRs), have been designed
Out.Due to its unique optical characteristics, by close attention, (for example, compared with zero dimension silicon nano, auger lifetime is more
Long, carrier multiplication quantum yield is higher.It has recently been demonstrated that the elongated nanostructure as nanometer rods may be shown
Special biobehavioral, such as quick tumour penetrate and enhance tumor accumulation (Nat.Rev.Mater.2016,1,16014;
Adv.Funct.Mater.2016,26,66-79;Small 2017,13,1604214;Biomaterials 2017,122,
188-200;Proc.Natl.Acad.Sci.USA 2008,105,11613-11618.).Therefore, unique optics and special life
Object behavioral trait makes fluorescence SiNRs hold promise for the nanometer therapeutic agent of cancer diagnosis and treatment, but still there are vacancies.
Although Recent study person prepares silicon nanostructure (such as: nano silicon particles, silicon nanowires, silicon nanorod in design
Deng) aspect achieves significant achievement, but designs novel silicon nanostructure and carry out simple, quick and be prepared into silicon at low cost
The important obstruction of Nano-technology Development.The glimmering of fluorescence and optoacoustic Photothermal Signals is had both about design however, there is no in the prior art
The report of light silicon nanorod.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of sides for preparing gold nano particle modification fluorescence silicon nanorod
Method, the function silicon nano material of this method preparation not only has good water dispersible, and has good fluorescence and photo-thermal
Characteristic can generate optoacoustic Photothermal Signals and be imaged for real-time biological.
To achieve the above object, for the present invention under the conditions of microwave radiation, gold ion is by growth in situ in fluorescence silicon nanorod
Surface obtains one-dimensional functionalized silicon nano material.
Specifically, the invention provides the following technical scheme:
The method for preparing gold nano particle modification fluorescence silicon nanorod of the invention, includes the following steps:
(1) silicon nanorod is formed into deionized water dispersion liquid, solution containing gold ion is added, be protected from light ultrasonic 30 minutes with
On, obtain precursor solution;
In above-mentioned technical proposal, the silicon nanorod diameter is 20~30 nanometers, length is 130~150 nanometers.
In above-mentioned technical proposal, the dispersion liquid concentration is 0.5~1g/ml.
In above-mentioned technical proposal, the solution containing gold ion is the chlorauric acid solution of 0.005~0.02M of concentration.
(2) precursor solution is put into microwave reactor and carries out microwave reaction;
In above-mentioned technical proposal, microwave reaction condition be 15~1000W of power, 100~150 DEG C of heating temperature, heating when
Between 60~120 minutes.
(3) solution that reaction is completed is cooled to room temperature, carries out centrifuge washing, obtained lower sediment is that target produces
Object.
In above-mentioned technical proposal, centrifuge washing condition is that centrifugal rotational speed is 14800 turns, 5 minutes every time, is repeated 3~4 times.
The fluorescence silicon nanorod size for the gold nano particle modification that the method for the present invention obtains is about 130~150 nanometers long, wide
About 20~30 nanometers, the partial size of gold nano grain is 5~10 nanometers, and photothermal conversion efficiency can achieve 44%, in ultraviolet light
It can be issued under the excitation of (365nm) blue-fluorescence (launch wavelength 455nm).The function silicon nano material has good optoacoustic
Response characteristic, with the increase of concentration, photoacoustce signal intensity enhancing;With good water dispersible, there is preferable fluorescent stabilization
Property and pH stability convert light energy into thermal energy under low-power 808nm laser irradiation to making solution temperature quickly increase.
In addition, the function silicon nano material can be used as fluorescent marker and contrast agent for biological detection and analysis, and it is expected into one
Step is applied to the diagnosis and treatment integration of multi-modality imaging guidance.
Detailed description of the invention
Fig. 1 is the transmission electron microscope of the silicon nanorod for the gold nano particle modification that the embodiment of the present invention 2 is prepared respectively
(TEM) figure (a)~b)), high-resolution-ration transmission electric-lens (HRTEM) figure (c)) and power spectrum (EDS) figure (d));
Fig. 2 is the fluorescence silicon nanorod and silicon nanometer for the gold nano particle modification that the embodiment of the present invention 2 is prepared respectively
Fluorescence (PL) spectrogram (a) of stick and gold nano grain) and ultraviolet-visible light (UV-Vis) abosrption spectrogram (b)) comparison diagram,
A) lower right corner is the fluorescence pictorial diagram being inserted into figure;
Fig. 3 is the photoacoustic imaging of the fluorescence silicon nanorod of the gold nano particle modification for the various concentration that the present invention is prepared
Scheme (a)) and photoacoustce signal intensity between linear relationship chart (b));
Fig. 4 is the fluorescence silicon nanorod for the gold nano particle modification that the embodiment of the present invention 2 is prepared in different capacity
Thermograph under 808 nm near-infrared laser irradiations;
In above-mentioned each attached drawing, SiNRs indicates that silicon nanorod, AuNPs indicate that gold nano grain, Au@SiNRs indicate gold nano
The fluorescence silicon nanorod of particle modification.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out detailed retouch
It states.
Raw material used in the present invention can freely be bought by market, be that analysis is pure;
Be used to prepare the microwave reactor model of gold nano particle modification silicon nanorod: NOVA-2S is purchased from Shanghai
Preekem company.
Embodiment 1
(1) 50 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.005M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 100W, 60 minutes heating times, 100 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 2
(1) 80 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.01M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 100W, 90 minutes heating times, 120 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 3
(1) 100 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.015M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 120W, 90 minutes heating times, 130 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 4
(1) 50 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.02M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 100W, 90 minutes heating times, 150 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 5
(1) 80 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.015M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 100W, 120 minutes heating times, 120 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 6
(1) 100 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.01M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 100W, 60 minutes heating times, 120 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 7
(1) 50 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.015M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 130W, 120 minutes heating times, 150 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 8
(1) 80 milligrams of silicon nanorods that be 20~30 nanometers by the diameter being prepared, length is 130~150 nanometers point
It is scattered in 10 milliliters of deionized water, the chlorauric acid solution of 100 microlitres of 0.02M is added, be protected from light ultrasound 30 minutes.
(2) obtained precursor solution is added in microwave reaction bottle, is put into microwave reactor and carries out microwave reaction, reacted
Condition is power 130W, 90 minutes heating times, 130 DEG C of heating temperature.
(3) material for obtaining reaction carries out centrifuge washing, and centrifugal rotational speed is 14800 turns, 5 minutes every time, repeats 3~4
Secondary, obtained lower sediment is target product.
By optic test, preparation-obtained material is used for optoacoustic and photothermal imaging.
Embodiment 2 is highly preferred embodiment of the present invention, learns the gold nano being prepared by the TEM figure of the embodiment 2 of Fig. 1
The silicon nanorod of particle modification has preferable dispersibility, about 130~150 nanometers long, about 20~30 nanometers wide, gold nano
The partial size of particle is 5~10 nanometers, finds out that gold nano grain and silicon nanorod all have clearly lattice, explanation from HRTEM figure
The fluorescence silicon nanorod for the gold nano particle modification being prepared has a good crystallinity, EDS map also secondary proof gold nano
The presence of particle.Fig. 2, which obtains UV-PL figure by embodiment 2, can be seen that the silicon nanorod for the gold nano particle modification being prepared
With apparent absorption peak and fluorescence emission peak.The optoacoustic photothermal imaging figure that Fig. 3 and Fig. 4 is obtained by embodiment 2 can be seen that system
The fluorescence silicon nanorod of standby obtained gold nano particle modification has excellent optical imagery performance.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (6)
1. a kind of method for preparing gold nano particle modification fluorescence silicon nanorod, which is characterized in that include the following steps;
S1, silicon nanorod is formed in deionized water to dispersion liquid, solution containing gold ion is added, be protected from light ultrasound 30 minutes or more,
Obtain precursor solution;
S2, it precursor solution is put into microwave reactor carries out microwave reaction;
S3, the solution that reaction is completed is cooled to room temperature, carries out centrifuge washing, obtained lower sediment is target product.
2. the method according to claim 1, wherein the silicon nanorod diameter is 20~30 nanometers, length is
130~150 nanometers.
3. the method according to claim 1, wherein the dispersion liquid concentration is 0.5~1g/ml.
4. the method according to claim 1, wherein the solution containing gold ion is 0.005~0.02M's of concentration
Chlorauric acid solution.
5. the method according to claim 1, wherein the microwave reaction condition is 15~1000W of power, heating
100~150 DEG C of temperature, 60~120 minutes heating times.
6. the method according to claim 1, wherein it is 14800 turns that the centrifuge washing condition, which is centrifugal rotational speed,
It 5 minutes every time, repeats 3~4 times.
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