CN105834451A - Preparation method for gold nanoparticle bipyramids - Google Patents
Preparation method for gold nanoparticle bipyramids Download PDFInfo
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- CN105834451A CN105834451A CN201610353418.XA CN201610353418A CN105834451A CN 105834451 A CN105834451 A CN 105834451A CN 201610353418 A CN201610353418 A CN 201610353418A CN 105834451 A CN105834451 A CN 105834451A
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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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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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
Abstract
The invention provides a preparation method for gold nanoparticle bipyramids. According to the method, chloroauric acid solutions are added into dodecyl trimethyl ammonium bromide solutions and sodium borohydride solutions for obtaining hydrosol of nanoscale gold particles, the hydrosol serves as seed solutions, and then the seed solutions are added into growth solutions for generating gold nanoparticle bipyramid particles; the preparation process is simple, the reaction condition is mild, and few cheap chemical reagents except for chloroauric acid are used.
Description
Technical field
The present invention relates to the preparation method of a kind of nano Au particle, particularly to the preparation method of a kind of gold nano bicone.
Background technology
Nanometer gold have uniqueness physicochemical properties and biological property, after surface modification obtain bio-imaging, photo-thermal therapy,
The abilities such as targeted drug conveying, have high potential using value in terms of the clinical diagnosis and treatment of cancer.With photo-thermal therapy
As a example by, owing to the double vertebral body of gold nano has the optical characteristics of uniqueness, surface plasma resonance phenomenon under certain condition, can be produced
(surface plasmon resonance, SPR), also can be converted to heat energy by the luminous energy of absorption, i.e. photothermal deformation effect.
The double vertebral body of gold nano with given shape has bigger specific surface area owing to comparing the double vertebral body of spherical gold nano, thus is subject to
Pay attention to, such as gold nanorods, gold nano star and gold nano triangle etc. to increasing.As a example by gold nanorods, can be by regulation
Fineness ratio is at the longitudinal SPR absworption peak of 800nm near infrared region (near infrared reflection, NIR) generation, and human body
Organize relatively weak to the absorption of this band of light, near-infrared laser therefore can be used to irradiate gold nanorods and realize tumor tissues
Molecular imaging, photo-thermal therapy and medicine controlled releasing, provide theoretical basis for its diagnosis and treatment being applied to cancer.
About all kinds of, there is the diplospondyly preparation method of given shape gold nano, existing more report, but double about gold nano
The report of cone is the most rare, and this synthetic method process is simple, and reaction condition is gentle, and the related reagent of use is relatively common.
Summary of the invention
The method of the preparation gold nano bicone that the present invention relates to, simple to operate and both economical, preparation cost is relatively low.
The technical scheme that the present invention provides comprises the following steps:
(1) the double vertebral body seed liquor of gold nano is prepared: be mixed to get bright by chlorauric acid solution and Dodecyl trimethyl ammonium chloride solution
Yellow liquid, adds sodium borohydride solution in described glassy yellow liquid and carries out reduction reaction, generates the double vertebral body of gold nano, obtains
The double vertebral body seed liquor of described gold nano；
(2) the double vertebral body growth-promoting media of gold nano is prepared: by chlorauric acid solution, hydrochloric acid solution and Dodecyl trimethyl ammonium chloride solution
After mixing, add silver nitrate solution and ascorbic acid solution, obtain the double vertebral body growth-promoting media of described gold nano；
(3) double for described gold nano vertebral body seed liquor are added to the double vertebral body growth-promoting media of described gold nano, give birth at a certain temperature
Grow up to gold nano bicone.
Wherein, step (3) also includes:
Under the temperature conditions of 20 DEG C～70 DEG C, generate gold nano bicone.
The most individual, in step (1):
The concentration of chlorauric acid solution, Dodecyl trimethyl ammonium chloride solution and sodium borohydride solution be respectively 0.005M～0.05M,
0.005～0.03M and 0.05M～2M.
Wherein, in step (1):
Sodium borohydride solution is now with the current, and sodium borohydride solution frozen water is prepared.
Wherein, step (1) also includes:
After generating the double vertebral body of gold nano, at 20 DEG C～30 DEG C, see that light stands 1h～2.5h and obtains the double vertebral body seed liquor of described gold nano.
Wherein, in step (2):
The concentration of chlorauric acid solution is 0.001M～0.01M, the concentration of Dodecyl trimethyl ammonium chloride solution is
0.004M～0.02M, the solubility of hydrochloric acid solution are 0.5M～1.5M, the concentration of ammonium nitrate solution is 0.005M～0.05M, anti-bad
The concentration of hematic acid solution is 0.05M～0.5M.
Wherein, in step (2):
Ascorbic acid solution needs now with the current.
Wherein, step (2) also includes:
After adding silver nitrate solution and ascorbic acid solution, see at 20 DEG C～70 DEG C that light places 6h～36h, obtain described gold nano double
Vertebral body growth-promoting media.
Wherein, step (3) also includes:
Wherein, the volume of the double vertebral body seed liquor of described gold nano is 30～100 μ L.
The preparation method of the present invention, has the advantages that
1, the preparation method of the present invention, simple to operate and both economical, preparation cost is relatively low.
2, the preparation method of the present invention, reaction quickly, mild condition, use to prepare reagent relatively common, and prepare
Gold nano bicone shape is regular.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of a kind of gold nano bicone of one embodiment of the present of invention；
Fig. 2 be a kind of gold nano bicone of one embodiment of the present of invention ultraviolet-visible light spectrogram；
Fig. 3 and Fig. 4 is the TEM image of gold nano bicone prepared by one embodiment of the present of invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
The preparation method 1 of 1 one kinds of gold nano bicones of embodiment
As it is shown in figure 1, specifically include following steps:
(1) the double vertebral body seed liquor of gold nano is prepared: by chlorauric acid solution and the dodecane of 7.5ml 0.1M of 0.25ml 0.01M
Base trimethylammonium bromide Solutions Solution mixes, and magnetic agitation 2min obtains glassy yellow liquid, adds 0.6ml in this glassy yellow liquid
The sodium borohydride solution of 0.01M, obtains brown solution, at 25 DEG C static 2 hours, obtains the double vertebral body seed liquor of gold nano.
(2) prepare the double vertebral body growth-promoting media of gold nano: take the chlorauric acid solution of 3ml 0.001M, the hydrochloric acid solution of 20 μ L 1M and
3ml 0.01M Dodecyl trimethyl ammonium chloride solution, gentle agitation obtains yellow solution, adds 40 μ L in this yellow solution
The silver nitrate solution of 0.01M and the ascorbic acid solution of 60 μ L 0.1M, under the conditions of 25 DEG C, be shown in that light is placed 25 hours, yellow
Solution gradually becomes colourless, prepares the double vertebral body growth-promoting media of gold nano.
(3) it is added to double for the gold nano of 60 μ L vertebral body seed liquor in the double vertebral body growth-promoting media of gold nano form mixed liquor, at 30 DEG C
Seeing that light is placed 24 hours, As time goes on, the color of mixed liquor is by colourless the most constant to peony again to pale pink to redness
Color, i.e. obtains gold nano bicone.
Fig. 2 is the ultraviolet-visible light spectrogram of the gold nano bicone prepared by preparation method 1, is wherein spherical at 535nm
The diplospondyly characteristic peak of gold nano, the absworption peak at 780nm is then the characteristic absorption peak of gold nano bicone, it was demonstrated that gold nano
Bicone synthesizes successfully.
Fig. 3 and Fig. 4 is the TEM image of the gold nano bicone made by preparation method 1.
The preparation method 2 of 2 one kinds of gold nano bicones of embodiment
Specifically include following steps:
(1) the double vertebral body seed liquor of gold nano is prepared: by molten to the chlorauric acid solution of 0.6ml 0.01M and DEG C TAB of 5ml 0.4M
Liquor mixes, and magnetic agitation 3min obtains glassy yellow liquid, adds the hydroboration of 0.6ml 0.1M in this glassy yellow liquid
Sodium solution, obtains brown solution, at 26 DEG C static 1.5 hours, obtains the double vertebral body seed liquor of gold nano.
(2) the double vertebral body growth-promoting media of gold nano is prepared: take the chlorauric acid solution of 4ml 0.003M, the hydrochloric acid solution of 10 μ L 0.1M
With 4ml 0.005M Dodecyl trimethyl ammonium chloride solution, gentle agitation obtains yellow solution, adds in this yellow solution
The silver nitrate solution of 60 μ L 0.006M and the ascorbic acid solution of 80 μ L 0.1M, under the conditions of 20 DEG C, be shown in that light is placed 6 hours
Yellow solution gradually becomes colourless, prepares the double vertebral body growth-promoting media of gold nano.
(3) it is added to double for the gold nano of 40 μ L vertebral body seed liquor in the double vertebral body growth-promoting media of gold nano form mixed liquor, at 35 DEG C
Seeing that light is placed 20 hours, growth-promoting media color again to peony to invariant color, is obtained gold nano bicone by colourless redness.
The preparation method 3 of 3 one kinds of gold nano bicones of embodiment
Specifically include following steps:
(1) the double vertebral body seed liquor of gold nano is prepared: by chlorauric acid solution and the dodecyl of 6ml 0.3M of 0.3ml 0.02M
Trimethylammonium bromide Solutions Solution mixes, and magnetic agitation 2min obtains glassy yellow liquid, adds 1ml in this glassy yellow liquid
The sodium borohydride solution of 0.05M, obtains brown solution, at 30 DEG C static 1 hour, obtains the double vertebral body seed liquor of gold nano.
(2) prepare the double vertebral body growth-promoting media of gold nano: take the chlorauric acid solution of 2ml 0.01M, the hydrochloric acid solution of 20 μ L 0.5M and
1ml 0.02M Dodecyl trimethyl ammonium chloride solution, gentle agitation obtains yellow solution, adds 40 μ L in this yellow solution
The silver nitrate solution of 0.01M and the ascorbic acid solution of 100 μ L 0.05M, under the conditions of 50 DEG C, be shown in that light is placed 16 hours, yellow
Color solution gradually becomes colourless, prepares the double vertebral body growth-promoting media of gold nano.
(3) it is added to double for the gold nano of 100 μ L vertebral body seed liquor in the double vertebral body growth-promoting media of gold nano form mixed liquor, at 40 DEG C
Under see light place 15 hours, As time goes on, the color of mixed liquor by colourless to pale pink again to peony, i.e. obtain gold
Nano double cone.
The preparation method 4 of 4 one kinds of gold nano bicones of embodiment
Specifically include following steps:
(1) the double vertebral body seed liquor of gold nano is prepared: by chlorauric acid solution and the dodecane of 7ml 0.15M of 0.25ml 0.04M
Base trimethylammonium bromide Solutions Solution mixes, magnetic agitation 2min, adds the boron hydrogen of 0.4ml 0.15M in this glassy yellow liquid
Change sodium solution, obtain brown solution, at 22 DEG C static 2 hours, obtain the double vertebral body seed liquor of gold nano.
(2) prepare the double vertebral body growth-promoting media of gold nano: take the chlorauric acid solution of 3ml 0.005M, the hydrochloric acid solution of 10 μ L 1M and
3ml 0.005M Dodecyl trimethyl ammonium chloride solution, gentle agitation obtains yellow solution, adds 50 μ L in this yellow solution
The silver nitrate solution of 0.02M and the ascorbic acid solution of 80 μ L 0.25M, gentle agitation stirring 60s, yellow solution gradually becomes
Colourless, prepare the double vertebral body growth-promoting media of gold nano.
(3) it is added to double for the gold nano of 80 μ L vertebral body seed liquor in the double vertebral body growth-promoting media of gold nano form mixed liquor, sees at 30 DEG C
Light place 18 hours, As time goes on, the color of mixed liquor by colourless to pale pink to redness again to peony, i.e. obtain
Gold nano bicone.
The preparation method 5 of 5 one kinds of gold nano bicones of embodiment
Specifically include following steps:
(1) the double vertebral body seed liquor of gold nano is prepared: by chlorauric acid solution and the dodecyl of 5ml 0.1M of 0.5ml 0.015M
Trimethylammonium bromide Solutions Solution mixes, and magnetic agitation 2min obtains glassy yellow liquid, adds 0.2ml in this glassy yellow liquid
The sodium borohydride solution of 0.2M, obtains brown solution, at 28 DEG C static 2 hours, obtains the double vertebral body seed liquor of gold nano.
(2) the double vertebral body growth-promoting media of gold nano is prepared: take the chlorauric acid solution of 5ml 0.001M, the hydrochloric acid solution of 20 μ L 0.8M
With 2ml 0.015M Dodecyl trimethyl ammonium chloride solution, gentle agitation obtains yellow solution, adds in this yellow solution
The silver nitrate solution of 40 μ L 0.01M and the ascorbic acid solution of 60 μ L 0.1M, under the conditions of 70 DEG C, be shown in that light is placed 36 hours,
Yellow solution gradually becomes colourless, prepares the double vertebral body growth-promoting media of gold nano.
(3) it is added to double for the gold nano of 45 μ L vertebral body seed liquor in the double vertebral body growth-promoting media of gold nano form mixed liquor, at 65 DEG C
See light place 6 hours, the color of mixed liquor by colourless to redness again to peony, i.e. obtain gold nano bicone.
In sum, the preparation method of the gold nano bicone of the present invention, have the advantages that
1, the preparation method of the present invention, simple to operate and both economical, preparation cost is relatively low.
2, the preparation method of the present invention, reaction quickly, mild condition, use to prepare reagent relatively common, and the gold nano prepared
Bicone shape is regular.
Claims (9)
1. the preparation method of a gold nano bicone, it is characterised in that comprise the following steps:
(1) the double vertebral body seed liquor of gold nano is prepared: be mixed to get bright by chlorauric acid solution and Dodecyl trimethyl ammonium chloride solution
Yellow liquid, adds sodium borohydride solution in described glassy yellow liquid and carries out reduction reaction, generates the double vertebral body of gold nano, obtains
The double vertebral body seed liquor of described gold nano；
(2) the double vertebral body growth-promoting media of gold nano is prepared: by chlorauric acid solution, hydrochloric acid solution and Dodecyl trimethyl ammonium chloride solution
After mixing, add silver nitrate solution and ascorbic acid solution, obtain the double vertebral body growth-promoting media of described gold nano；
(3) double for described gold nano vertebral body seed liquor are added to the double vertebral body growth-promoting media of described gold nano, give birth at a certain temperature
Grow up to gold nano bicone.
2. the preparation method of gold nano bicone as claimed in claim 1, it is characterised in that described step (3) also includes:
Under the temperature conditions of 20 DEG C～70 DEG C, generate gold nano bicone.
3. the preparation method of gold nano bicone as claimed in claim 1, it is characterised in that in described step (1):
The concentration of chlorauric acid solution, Dodecyl trimethyl ammonium chloride solution and sodium borohydride solution be respectively 0.005M～0.05M,
0.005～0.03M and 0.05M～2M.
4. the preparation method of the gold nano bicone as described in claim 1 or 3, it is characterised in that in described step (1):
Sodium borohydride solution is now with the current, and sodium borohydride solution frozen water is prepared.
5. the preparation method of gold nano bicone as claimed in claim 1, it is characterised in that described step (1) also includes:
After generating the double vertebral body of gold nano, at 20 DEG C～30 DEG C, see that light stands 1h～2.5h and obtains the double vertebral body seed liquor of described gold nano.
6. the preparation method of gold nano bicone as claimed in claim 1, it is characterised in that in described step (2):
The concentration of chlorauric acid solution is 0.001M～0.01M, the concentration of Dodecyl trimethyl ammonium chloride solution is
0.004M～0.02M, the solubility of hydrochloric acid solution are 0.5M～1.5M, the concentration of ammonium nitrate solution is 0.005M～0.05M, anti-bad
The concentration of hematic acid solution is 0.05M～0.5M.
7. the preparation method of the gold nano bicone as described in claim 1 or 6, it is characterised in that in described step (2):
Ascorbic acid solution needs now with the current.
8. the preparation method of gold nano bicone as claimed in claim 1, it is characterised in that described step (2) also includes:
After adding silver nitrate solution and ascorbic acid solution, see at 20 DEG C～70 DEG C that light places 6h～36h, obtain described gold nano double
Vertebral body growth-promoting media.
9. the preparation method of gold nano bicone as claimed in claim 1, it is characterised in that described step (3) also includes:
Wherein, the volume of the double vertebral body seed liquor of described gold nano is 30～100 μ L.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077705A (en) * | 2016-08-19 | 2016-11-09 | 东华大学 | A kind of preparation method of gold nanorods |
| CN107175338A (en) * | 2017-04-10 | 2017-09-19 | 广东工业大学 | A kind of trigonal biyramid palladium list twin and its preparation method and application |
| CN108161020A (en) * | 2016-12-13 | 2018-06-15 | 中国科学院光电技术研究所 | A kind of octahedral preparation method of gold nano |
| CN109396457A (en) * | 2018-12-05 | 2019-03-01 | 武汉大学苏州研究院 | A kind of shape and the controllable nanogold particle and the preparation method and application thereof of size |
| CN109489854A (en) * | 2018-12-27 | 2019-03-19 | 中国科学院理化技术研究所 | A kind of nanogold cone photothermal reagent and preparation method thereof with temp sensing function |
| CN110340348A (en) * | 2019-08-05 | 2019-10-18 | 郴州市金贵银业股份有限公司 | A kind of nano-silver powder, preparation method, silver paste and application |
| CN114309636A (en) * | 2021-12-28 | 2022-04-12 | 江南大学 | Chiral gold nano antibacterial material and preparation method thereof |
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| CN104907578A (en) * | 2015-04-29 | 2015-09-16 | 福州大学 | Method for preparing gold nanorods |
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| US20100239675A1 (en) * | 2009-03-20 | 2010-09-23 | Northwestern University | Plasmon mediated photoinduced synthesis of silver triangular bipyramids |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077705A (en) * | 2016-08-19 | 2016-11-09 | 东华大学 | A kind of preparation method of gold nanorods |
| CN108161020A (en) * | 2016-12-13 | 2018-06-15 | 中国科学院光电技术研究所 | A kind of octahedral preparation method of gold nano |
| CN107175338A (en) * | 2017-04-10 | 2017-09-19 | 广东工业大学 | A kind of trigonal biyramid palladium list twin and its preparation method and application |
| CN107175338B (en) * | 2017-04-10 | 2019-04-19 | 广东工业大学 | A kind of trigonal biyramid palladium list twin and its preparation method and application |
| CN109396457A (en) * | 2018-12-05 | 2019-03-01 | 武汉大学苏州研究院 | A kind of shape and the controllable nanogold particle and the preparation method and application thereof of size |
| CN109396457B (en) * | 2018-12-05 | 2022-02-15 | 武汉大学苏州研究院 | Shape and size controllable gold nanoparticle and preparation method and application thereof |
| CN109489854A (en) * | 2018-12-27 | 2019-03-19 | 中国科学院理化技术研究所 | A kind of nanogold cone photothermal reagent and preparation method thereof with temp sensing function |
| CN109489854B (en) * | 2018-12-27 | 2020-09-18 | 中国科学院理化技术研究所 | Nano gold cone photo-thermal reagent with temperature measurement function and preparation method thereof |
| CN110340348A (en) * | 2019-08-05 | 2019-10-18 | 郴州市金贵银业股份有限公司 | A kind of nano-silver powder, preparation method, silver paste and application |
| CN110340348B (en) * | 2019-08-05 | 2021-12-21 | 郴州市金贵银业股份有限公司 | Nano silver powder, preparation method, silver paste and application |
| CN114309636A (en) * | 2021-12-28 | 2022-04-12 | 江南大学 | Chiral gold nano antibacterial material and preparation method thereof |
| CN114309636B (en) * | 2021-12-28 | 2024-01-19 | 江南大学 | Chiral gold nano antibacterial material and preparation method thereof |
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