CN113547130A - Laser-assisted functionalized gold nano-star preparation method - Google Patents
Laser-assisted functionalized gold nano-star preparation method Download PDFInfo
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 34
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 26
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 13
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 13
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 13
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 6
- 239000012498 ultrapure water Substances 0.000 claims abstract description 6
- 229910004042 HAuCl4 Inorganic materials 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 230000001678 irradiating effect Effects 0.000 claims abstract description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000000020 Nitrocellulose Substances 0.000 claims description 5
- 229920001220 nitrocellulos Polymers 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000010931 gold Substances 0.000 description 15
- 229910052737 gold Inorganic materials 0.000 description 12
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- 239000002245 particle Substances 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 5
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- 230000005540 biological transmission Effects 0.000 description 4
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- 230000008859 change Effects 0.000 description 3
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
Abstract
The invention relates to a preparation method of laser-assisted functionalized gold nano-star, which comprises the following steps: (1) under stirring in HAuCl4Adding HCl and AgNO into the solution in sequence3And ascorbic acid to obtain a dark green mixed solution A; (2) adding the mixed solution B into the mixed solution A, then irradiating by using laser, and standing in the dark after irradiation is finished to obtain a mixed solution C; wherein the mixed solution B consists of equal volume of K2CO3Solution and HS- (O-CH)2‑CH 2)n‑(CH2)2-COOH in admixture(ii) a (3) And dispersing the mixed solution C in ultrapure water, and then filtering to obtain the gold nano-star. Compared with the prior art, the preparation method provided by the invention does not need to synthesize a seed solution, and can synthesize the functionalized gold nano-star in one step under the assistance of laser at normal temperature, so that the synthesis of the gold nano-star is simpler and faster.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of laser-assisted functionalized gold nano-star.
Background
Gold nanostars (GNSt) are gold nanoparticles with sharp peaks protruding from the spherical core. Compared to other gold nanoparticles, the sharp peaks can promote strong Local Surface Plasmon Resonance (LSPR) of the nanoparticles in the region of the spectrum from red to near infrared. Strong LSPR can produce local electric field enhancement at the tip of the spike, between individual gold nanostar spikes, and between adjacent gold nanostar spikes. These characteristics are that gold nano-star becomes a research hotspot in the field of plasma. In addition, when the gold nanoparticles are small enough, the gold nanoparticles can conveniently enter cells, and have great prospect in the field of biomedicine. The gold nano-star particles with good biocompatibility have great potential in the fields of biochemical analysis, biosensing, diagnosis and treatment and the like.
The synthesis of the gold nanostar generally requires two steps, namely, the gold nanosphere seed solution is synthesized, and then the gold nanospheres in the seed solution are used as cores to grow into the gold nanostar particles. In addition, the process of synthesizing the gold nano-star usually needs heating, so the operation is very inconvenient; the use of surfactants increases cytotoxicity, which greatly limits their use in biomedicine.
Therefore, there is an urgent need in the art for a method for preparing gold nano-star that is simpler and faster to synthesize and does not use a surfactant.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of laser-assisted functionalized gold nano-stars.
In a first aspect, the present application provides a method for preparing laser-assisted functionalized gold nano-star, comprising the following steps:
(1) under stirring in HAuCl4Adding HCl and AgNO into the solution in sequence3And ascorbic acid to obtain a dark green mixed solution A;
(2) adding the mixed solution B into the mixed solution A, then irradiating by using laser, and standing in the dark after irradiation is finished to obtain a mixed solution C; wherein the mixed solution B consists of equal volume of K2CO3Solution and HS- (O-CH)2-CH 2)n-(CH2)2-COOH;
(3) and dispersing the mixed solution C in ultrapure water, and then filtering to obtain the gold nano-star.
In the step (1), HCl adjusts the pH value of the solution; ascorbic acid as a reducing agent, AgNO3Assisting the formation of gold nano-stars. In an acidic environment, ascorbic acid is in AgNO3With the aid of (2) Au3+Reduction to Au0And in Ag+With the assistance of (2), the gold nano-star particles are grown.
In step (2), K2CO3Adding HS- (O-CH) for adjusting the pH of the solution to be alkalescent2-CH2)n-(CH2)2The addition of-COOH (i.e. PEG) is used for the functionalization of gold nano-star particles, and the PEG forms Au-S bonds with the Au surface.
In the step (3), (3) laser irradiates on the surface of the gold nano-star particles to form Surface Plasmon Resonance (SPR), so that the local temperature is increased, and the surface functionalization of the gold nano-particles is facilitated and accelerated.
In one embodiment of the first aspect, in step (1), the HAuCl is4、HCl、AgNO3And the molar ratio of the ascorbic acid is (300-600): (2000-4000): (1-5): (500-1500).
In one embodiment of the first aspect, in the step (1), the stirring rate is 500 to 1000 rpm.
In one embodiment of the first aspect, in step (2), K in the mixed solution B2CO3The molar concentration of (b) is 1 to 3 mM.
In one embodiment of the first aspect, in step (2), the K is added2CO3With HAuCl4The molar ratio of (30-50): (300-600).
In one embodiment of the first aspect, in step (2), the HS- (O-CH)2-CH2)n-(CH2)2The relative molecular mass of-COOH is 1.8-2.5 kDa.
In one embodiment of the first aspect, in the step (2), the wavelength of the laser is 600 to 900nm, the power is 5 to 10w, and the irradiation area of the laser is 4 to 6cm2(ii) a The irradiation mode of the laser is as follows: irradiating every 4-6 min for 25-40 s each time for 2-5 times. (4) Laser irradiates on the surface of the gold nano-star particles to form Surface Plasmon Resonance (SPR), so that the local temperature is raised, and the surface functionalization of the gold nano-particles is facilitated and accelerated. The continuous laser is used for assisting the gold nano-star functionalization, so that the local high temperature of the surface of a gold nano-star particle is ensured, the higher energy required by the functionalized macromolecules to form Au-S bonds on the surface of gold is met, the functionalization efficiency is higher, and the repeated irradiation is used for preventing the surface of the gold nano-particle from being melted due to overhigh local temperature, so that functional molecules are separated from the surface of the gold. The laser with the wavelength of 600 plus 900nm is used, the wavelength of the laser source is consistent in the range of the absorption peak of the gold nano-particles, the laser absorption efficiency is favorably improved, and the local temperature rise is accelerated.
In one embodiment of the first aspect, in the step (2), the standing time is 0.5-2 h.
In one embodiment of the first aspect, in step (3), the conditions used for the dispersion are as follows: the dispersion temperature is 3-8 ℃, the centrifugal speed is 3000-5000 rpm, and the dispersion time is 10-20 min.
In one embodiment of the first aspect, in step (3), the membrane used for filtration is a nitrocellulose membrane having a pore size of 0.22 μm.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method adopts a one-step method to synthesize the gold nano-star, does not need to synthesize a seed solution, and has the advantages of simple and rapid operation, strong repeatability and low cost;
(2) the reaction can be carried out at normal temperature without heating, and the reaction condition is mild;
(3) the preparation method does not need to use a surfactant, and has good biocompatibility.
Drawings
FIG. 1 is a UV-Vis absorption spectrum of the gold nanostar prepared in example 1;
FIG. 2 is a transmission electron micrograph of the gold nanostars prepared in example 2.
Detailed Description
Unless otherwise indicated, implied from the context, or customary in the art, all parts and percentages herein are by weight and the testing and characterization methods used are synchronized with the filing date of the present application. Where applicable, the contents of any patent, patent application, or publication referred to in this application are incorporated herein by reference in their entirety and their equivalent family patents are also incorporated by reference, especially as they disclose definitions relating to synthetic techniques, products and process designs, polymers, comonomers, initiators or catalysts, and the like, in the art. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
The numerical ranges in this application are approximations, and thus may include values outside of the ranges unless otherwise specified. A numerical range includes all numbers from the lower value to the upper value, in increments of 1 unit, provided that there is a separation of at least 2 units between any lower value and any higher value. For example, if a component, physical or other property (e.g., molecular weight, etc.) is recited as 100 to 1000, it is intended that all individual values, e.g., 100, 101,102, etc., and all subranges, e.g., 100 to 166,155 to 170,198 to 200, etc., are explicitly recited. For ranges containing a numerical value less than 1 or containing a fraction greater than 1 (e.g., 1.1, 1.5, etc.), then 1 unit is considered appropriate to be 0.0001, 0.001, 0.01, or 0.1. For ranges containing single digit numbers less than 10 (e.g., 1 to 5), 1 unit is typically considered 0.1. These are merely specific examples of what is intended to be expressed and all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be expressly stated in this application. It should also be noted that the terms "first," "second," and the like herein do not define a sequential order, but merely distinguish between different structures.
When used with respect to chemical compounds, the singular includes all isomeric forms and vice versa (e.g., "hexane" includes all isomers of hexane, individually or collectively) unless expressly specified otherwise. In addition, unless explicitly stated otherwise, the use of the terms "a", "an" or "the" are intended to include the plural forms thereof.
The terms "comprising," "including," "having," and derivatives thereof do not exclude the presence of any other component, step or procedure, and are not intended to exclude the presence of other elements, steps or procedures not expressly disclosed herein. To the extent that any doubt is eliminated, all compositions herein containing, including, or having the term "comprise" may contain any additional additive, adjuvant, or compound, unless expressly stated otherwise. Rather, the term "consisting essentially of … …" excludes any other components, steps or processes from the scope of any of the terms hereinafter recited, except those necessary for performance. The term "consisting of … …" does not include any components, steps or processes not specifically described or listed. Unless explicitly stated otherwise, the term "or" refers to the listed individual members or any combination thereof.
Examples
The following will describe in detail the embodiments of the present invention, which are implemented on the premise of the technical solution of the present invention, and the detailed embodiments and the specific operation procedures are given, but the scope of the present invention is not limited to the following embodiments.
Example 1
A preparation method of laser-assisted functionalized gold nano-star comprises the following steps:
(1) 300 μ L of 1M HCl was added to 200mL of 2.5 at 800rpm with stirring×10-4MHAuCl4To the solution, 20. mu.L of 0.01M AgNO was added3Solution, then, 1mL of 0.1M AA (Ascorbic Acid) solution was added quickly. The solution was observed to change rapidly from a bright red to a dark green color.
(2) 2mL of 2mM K mixed in equal volume was added2CO3And HS- (O-CH)2-CH2)n-(CH2)2-COOH (molecular weight 2kDa) mixed solution. Then, a continuous laser (DenLase-810/7, Beijing China, wavelength 808nm, power 6W, laser irradiation area 5 cm)2) Irradiation was carried out for 30S, once every 5 minutes, for three times. After the irradiation was completed, the plate was left standing in the dark.
(3) After one hour, the solution was centrifuged at 4000rpm for 15min at 4 ℃ and redispersed in ultrapure water. Finally, the solution was filtered through a nitrocellulose membrane having a pore size of 0.22 μm and stored in a refrigerator at 4 ℃.
The prepared gold nano-star is detected, and the UV-Vis absorption spectrum and the transmission electron microscope spectrum of the gold nano-star are respectively shown in figures 1 and 2.
Fig. 1 shows a UV-Vis spectrum of a gold nanostar solution formed by an embodiment of the present invention. As can be seen from fig. 1, the absorbance peak of the solution occurred at a wavelength of 743nm, thereby verifying the effectiveness of the embodiment of the present invention.
Fig. 2 shows a transmission electron microscope TEM image of gold nanorods formed by an embodiment of the present invention. As can be seen from fig. 2, the formed gold nanostar structure has the characteristics of a core and a branch structure. The diameter of the gold nano star core formed by the method in the embodiment of the invention is 42 +/-6 nm, the length of the branch structure is within the range of 8 +/-4 nm, and the number of branches is within the range of 6 +/-6.
Therefore, the method for preparing the gold nano-star by the one-step method at normal temperature without using a surfactant or synthesizing a seed solution is simple and rapid to operate, high in repeatability and low in cost.
Example 2
(1) 200 μ L of 1M HCl was added to 100 with stirring at 500rpmmL 3.0×10-4MHAuCl4To the solution, 20. mu.L of 0.025M AgNO was added3Solution, then, 0.5mL of 0.1M AA (Ascorbic Acid) solution was added quickly. The solution was observed to change rapidly from a bright red to a dark green color.
(2) 5mL of 1mM K mixed in equal volume was added2CO3And HS- (O-CH)2-CH2)n-(CH2)2-COOH (molecular weight 1.8kDa) mixed solution. Then, a continuous laser (DenLase-810/7, Beijing China, wavelength 600nm, power 5W, laser irradiation area 6 cm)2) Irradiation was carried out for 25S, once every 4 minutes, for 5 times. After the irradiation was completed, the plate was left standing in the dark.
(3) After 0.5 hour, the solution was centrifuged at 5000rpm for 20min at 3 ℃ and redispersed in ultrapure water. Finally, the solution was filtered through a nitrocellulose membrane having a pore size of 0.22 μm and stored in a refrigerator at 3 ℃.
The gold nano star is successfully synthesized by UV-Vis spectrum and transmission electron microscope scanning detection, the core diameter of the gold nano star is 40 +/-5 nm, the length of the branch structure is within the range of 7 +/-3.5 nm, and the number of branches is within the range of 7 +/-5.
Example 3
(1) 200 μ L of 2M HCl was added to 200mL of 3.0X 10 at 1000rpm with stirring-4MHAuCl4To the solution, 10. mu.L of 0.01M AgNO was added3Solution, then, 1.5mL of 0.1M AA (Ascorbic Acid) solution was added quickly. The solution was observed to change rapidly from a bright red to a dark green color.
(2) 1.5mL of 2mM K mixed in equal volume was added2CO3And HS- (O-CH)2-CH2)n-(CH2)2-COOH (molecular weight 2.5kDa) mixed solution. Then, a continuous laser (DenLase-810/7, Beijing China, wavelength 900nm, power 10W, laser irradiation area 4 cm)2) Irradiation was carried out for 40S, once every 6 minutes for 2 times. After the irradiation was completed, the plate was left standing in the dark.
(3) After two hours, the solution was centrifuged at 3000rpm for 10min at 8 ℃ and redispersed in ultrapure water. Finally, the solution was filtered through a nitrocellulose membrane having a pore size of 0.22 μm and stored in a refrigerator at 4 ℃.
The gold nano star is successfully synthesized by UV-Vis spectrum and transmission electron microscope scanning detection, the core diameter of the gold nano star is 43 +/-6 nm, the length of a branch structure is within the range of 8 +/-4.5 nm, and the number of branches is within the range of 6 +/-5.
The embodiments described above are intended to facilitate the understanding and appreciation of the application by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present application is not limited to the embodiments herein, and those skilled in the art who have the benefit of this disclosure will appreciate that many modifications and variations are possible within the scope of the present application without departing from the scope and spirit of the present application.
Claims (10)
1. A preparation method of laser-assisted functionalized gold nano-star is characterized by comprising the following steps:
(1) under stirring in HAuCl4Adding HCl and AgNO into the solution in sequence3And ascorbic acid to obtain a dark green mixed solution A;
(2) adding the mixed solution B into the mixed solution A, then irradiating by using laser, and standing in the dark after irradiation is finished to obtain a mixed solution C; wherein the mixed solution B consists of equal volume of K2CO3Solution and HS- (O-CH)2-CH 2)n-(CH2)2-COOH;
(3) and dispersing the mixed solution C in ultrapure water, and then filtering to obtain the gold nano-star.
2. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in step (1), the HAuCl is added4、HCl、AgNO3And the molar ratio of the ascorbic acid is (300-600): (2000-4000): (1E >5)：(500～1500)。
3. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in the step (1), the stirring speed is 500-1000 rpm.
4. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in the step (2), K in the mixed solution B2CO3The molar concentration of (b) is 1 to 3 mM.
5. The method for preparing laser-assisted functionalized gold nanostars as claimed in claim 4, wherein in step (2), the K is added2CO3With HAuCl4The molar ratio of (30-50): (300-600).
6. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in step (2), the HS- (O-CH)2-CH 2)n-(CH2)2The relative molecular mass of-COOH is 1.8-2.5 kDa.
7. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in the step (2), the wavelength of the laser is 600 to 900nm, the power of the laser is 5 to 10w, and the irradiation area of the laser is 4 to 6cm2；
The irradiation mode of the laser is as follows: irradiating every 4-6 min for 25-40 s each time for 2-5 times.
8. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in the step (2), the standing time is 0.5 to 2 hours.
9. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in the step (3), the dispersion is carried out under the following conditions: the dispersion temperature is 3-8 ℃, the centrifugal speed is 3000-5000 rpm, and the dispersion time is 10-20 min.
10. The method for preparing laser-assisted functionalized gold nanostars according to claim 1, wherein in the step (3), the membrane used for filtration is a nitrocellulose membrane with a pore size of 0.22 μm.
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