CN108145176A - A kind of autoreduction preparation method of gold nano ball-bar polymer - Google Patents
A kind of autoreduction preparation method of gold nano ball-bar polymer Download PDFInfo
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- CN108145176A CN108145176A CN201810022166.1A CN201810022166A CN108145176A CN 108145176 A CN108145176 A CN 108145176A CN 201810022166 A CN201810022166 A CN 201810022166A CN 108145176 A CN108145176 A CN 108145176A
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- 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
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Abstract
The invention discloses a kind of autoreduction preparation methods of gold nano bat polymer, and synthesis step is simple, and it is good to prepare effect.The present invention only can synthesize bat polymer in the synthesis process without introducing new Jin Yuan or gold nanosphere into stoste by a step phase conversion method.In addition, the experimental method efficient quick, experimental cost is also reduced while simplifying experimental procedure.Importantly, present invention eliminates ball present in other common methods and sticks to change the complex steps that chain links again respectively, conventional efficient is substantially increased.The bat polymer that the present invention prepares not only realizes large area preparation, but also absorption peak either still all has extraordinary application prospect and researching value in Raman image near infrared region in photo-thermal therapy field.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of autoreduction of gold nano ball-bar polymer
Preparation method.The present invention can be used for the preparation of gold nano ball-bar polymer.
Background technology
Unique surface plasmon resonance characteristic, good stability and bio-compatible possessed by gold nanorods
Property makes it in medical imaging and drug delivery, optical data storage, sensor, Surface enhanced Raman scattering, particularly in tumour
It suffers from being widely applied in terms of photo-thermal therapy, have been a concern for many years.However, the swift and violent hair with modern nanometer technology
Exhibition, new application propose higher requirement to the design of new material with preparation.Although gold nanorods receive always for a long time
Favor, but the physical property research of monomer stick and application encounter bottleneck, people start to turn to sight with monomer nanometer material
Expect for basic unit, to construct a nanometer multimeric structure by assembling multimerization nano single material, this becomes rises instantly
Research hotspot.
Nanometer the most significant feature of polymer be：When nanoparticle aggregate, it is hot that many tips and inflection point etc. can be generated
Point position, their electronic resonance is coupled due to strong electromagnetic interaction, so as to excite Plasmon Resonance.It is this
Resonance coupling brings novel characteristic：Energy of electromagnetic field is greatly converged to the aperture of coupled structure, i.e., most
Energy of electromagnetic field in one only several nanometers of small space, so as to bring huge Electromagnetic enhancement, is much larger than by local
The local field strength of monomer nano particle.Therefore, nanometer polymer receives the fervent concern of researchers, especially with gold nano
Ball-bar couples polymer for the Plasmon Resonance of representative, is with a wide range of applications and researching value.
Patent of invention " the Controllable assembly method of plasmon baseball ' corn ' structure " (Shen of Nanjing Univ. of Posts and Telecommunications's application
Please number：201510142694.7 application publication number：104858445 A of CN) in disclose and a kind of prepare plasmon baseball
The method of " corn " structure, the invention are first respectively to synthesize, then change chain respectively ball, stick, are finally mixed to get ball-bar " corn "
Structure.It is allowed to ultimately form ball-bar assembly by the response parameter for adjusting each step.Deficiency existing for the patented technology
Place is：It needs to prepare gold nanorods and gold nano grain respectively, other synthesized micromolecule is additionally wanted, then respectively to gold nano
Stick and gold nanosphere are surface modified, and not only the time used is long but also conventional efficient is low for this method, can be obtained by its attached drawing
Know that the method does not have evidence to prove that it can synthesize the ball-bar of large area " corn " structure polymer.
A kind of patent of invention " side that based on self-assembled material cancer cell surfaces are enhanced with Raman detection of Southern Yangtze University's application
Method " (application number：201110174033, Authorization Notice No.：A kind of self-assembled material that is based on is disclosed in 102346148B) to cancer
The method that cell surface enhances Raman detection is prepared, gold nanorods including gold nanorods probe and gold nanoparticle probe
The self assembly of probe and gold nanoparticle probe, surface-enhanced Raman detection cancer cell.Shortcoming existing for the patented technology
It is：Gold nanoparticle is being prepared around during gold nanorods are assembled into satellite-type structure, in addition to preparing gold nanorods and right
It outside it is modified, also in addition to prepare gold nanosphere and it is modified, can be seen that it is not synthesized by its attached drawing in addition
Go out large-area ordered polymer, the experimental procedure of very complicated greatly limits the actual use of this method.It would therefore be highly desirable to it carries
Go out a kind of method that step simply prepares large-area ordered assembly.
Invention content
The purpose of the present invention is overcoming the shortcoming of above-mentioned gold nano ball-bar poly preparation, a kind of gold is proposed
The autoreduction preparation method of nanometer ball-bar polymer.The present invention can be used to provide it is a kind of easy to operate, without in addition preparing Jenner
The ball-bar poly preparation of rice ball.
Realizing the thinking of the object of the invention is, the uniform gold nanorods of the pattern prepared are passed through a step and turned by the present invention
Phase method prepares large area ball-bar nanometer polymer.
Realize the specific steps of the object of the invention including as follows：
(1) synthesis of seed liquor：
The three hydration tetra chlorauric acid solution of a concentration of 0.5mM of 2.5mL are placed in 20mL vials by (1a), are added in thereto
The cetyl trimethylammonium bromide solution of a concentration of 0.2M of 2.5mL, solution colour become yellowish-brown by colourless, obtain solution A；
A concentration of 0.01M sodium borohydride solutions of 0.3mL are diluted with water 0.5mL by (1b), are rapidly injected solution A, solution
Color becomes light brown from yellowish-brown immediately, and continues strong stirring 2min, obtains solution B；
(1c) by solution B under the conditions of 30 DEG C about 3 hours of aging to get seed liquor；
(2) synthesis of growth-promoting media：
0.617g enuatrols and 4.5g cetyl trimethylammonium bromides are placed in 500mL conical flasks by (2a), thereto
Add in the hot water of about 50 DEG C of 125mL.Stirring makes it naturally cool to 30 DEG C, obtains solution C；
(2b) adds in the silver nitrate solution of a concentration of 4mM of 9mL to solution C, stops stirring, it is made to be stood in 30 DEG C of constant temperature
15min obtains solution D；
(2c) adds in the three hydration tetra chlorauric acid solution of a concentration of 1mM of 125mL into solution D, stirs 90min, Ran Houzai
The hydrochloric acid stirring 15min of a concentration of 12.1M of 0.75mL is added in, obtains solution E；
(2d) adds in the ascorbic acid solution of 0.625mL a concentration of 0.064mM into solution E, strong stirring 30s to get
Growth-promoting media；
(3) synthesis of the gold nanorods of double base surfactant cladding：
(3a) takes 0.2mL seed liquors, is rapidly injected in growth-promoting media, strong stirring 30s；
(3b) stands aging 22h to get gold nanorods solution in 30 DEG C of constant temperature；
(4) acquisition of gold nanorods pure water solution：
The good gold nanorods solution of the aging obtained in (3b) is centrifuged 20min by (4a) under 9000rpm, makes gold nanorods
Sink to centrifugation bottom of the tube；
(4b) is according to 1：1 volume ratio disperses centrifuge tube bottom precipitation in deionized water, to obtain gold nanorods again
Pure water solution；
(5) synthesis of ball-bar polymer：
(5a) takes the gold nanorods solution 3mL obtained in (4b), adds in 3mL concentration thereto under conditions of strong stirring
For 10mM thiomalic acid aqueous solutions；
(5b) adds in sodium hydrate aqueous solution thereto, and solution ph is transferred to 9.5；
(5c) adds in the o-dichlorobenzene solution of a concentration of tetra- n-octyl ammonium bromides of 50mM of 1.5mL, strong stirring thereto
After 30min, by solution left standstill for a period of time, you can observe that solution is significantly layered.Supernatant liquor is shifted, leaves bottom powder
Color solution is ball-bar poly liquid solution.
Compared with the prior art, the present invention has the following advantages:
First, the present invention only directly can synthesize ball-bar polymer by a step phase conversion method by gold nanorods, no
Only without in addition synthesizing gold nanosphere, and in the synthesis process without introducing new Jin Yuan into stoste.So as to reduce reality
Cost is tested, simplifies experimental procedure, substantially increases the combined coefficient of experiment.
Second, " one kind is based on self assembly material for the patented technology possessed present invention eliminates Southern Yangtze University of the prior art
Expect the method to cancer cell surfaces enhancing Raman detection " (application number：201110174033, Authorization Notice No.：102346148B)
Patented technology " the Controllable assembly method of plasmon baseball ' corn ' the structure " (application number possessed with Nanjing Univ. of Posts and Telecommunications：
201510142694.7 application publication number：104858445 A of CN) in during self-assembled material is prepared existing ball and stick
The complex steps that chain links again are changed respectively.
Third, the ball-bar poly bulk area that the present invention prepares is big, and in biologic applications, Raman enhancing etc. has very
Big application potential.
Description of the drawings
Fig. 1 is the gold nanorods in the present invention obtained in step (4) and ball-stick polymer obtained in step (5)
Absorption spectrum photo.
Fig. 2 is the transmission electron microscope photo of the gold nanorods obtained in step (4) in the present invention.
Fig. 3 is the transmission electron microscope photo of the ball-bar polymer obtained in step (5) in the present invention.
Fig. 4 is in the ball-bar polymer in the present invention obtained in step (5), and the transmission electron microscope of fine structure shines
Piece.
Specific embodiment
Step 1, the synthesis of seed liquor：
The three hydration tetra chlorauric acid solution of a concentration of 0.5mM of 2.5mL are placed in 20mL vials, are added in thereto
The cetyl trimethylammonium bromide solution of a concentration of 0.2M of 2.5mL, solution colour become yellowish-brown by colourless, obtain solution A；
A concentration of 0.01M sodium borohydride solutions of 0.3mL are diluted with water 0.5mL, are rapidly injected solution A, solution colour
Light brown is become from yellowish-brown immediately, and continues strong stirring 2min, obtains solution B；
By solution B under the conditions of 30 DEG C about 3 hours of aging to get seed liquor；
Step 2, the synthesis of growth-promoting media：
0.617g enuatrols and 4.5g cetyl trimethylammonium bromides are placed in 500mL conical flasks, added in thereto
The hot water that about 50 DEG C of 125mL.Stirring makes it naturally cool to 30 DEG C, obtains solution C；
The silver nitrate solution of a concentration of 4mM of 9mL is added in solution C, stops stirring, it is made to stand 15min in 30 DEG C of constant temperature,
Obtain solution D；
The three hydration tetra chlorauric acid solution of a concentration of 1mM of 125mL are added in into solution D, 90min is stirred, then adds
The hydrochloric acid stirring 15min of a concentration of 12.1M of 0.75mL, obtains solution E；
The ascorbic acid solution of a concentration of 0.064mM of 0.625mL is added in into solution E, strong stirring 30s is to get growth
Liquid；
Step 3, the synthesis of the gold nanorods of double base surfactant cladding：
0.2mL seed liquors are taken, are rapidly injected in growth-promoting media, strong stirring 30s；
Aging 22h is stood to get gold nanorods solution in 30 DEG C of constant temperature；
Step 4, the preparation of gold nanorods pure water solution：
The good gold nanorods solution of aging is centrifuged into 20min under 9000rpm, gold nanorods is made to sink to centrifugation bottom of the tube；
According to 1：1 volume ratio disperses centrifuge tube bottom precipitation in deionized water, to obtain gold nanorods pure water again
Solution；
Step 5, the synthesis of bat polymer：
Gold nanorods solution 3mL is taken, adds in a concentration of 10mM thiomalic acids of 3mL thereto under conditions of strong stirring
Aqueous solution；
Sodium hydrate aqueous solution is added in thereto, and solution ph is transferred to 9.5；
The o-dichlorobenzene solution of a concentration of tetra- n-octyl ammonium bromides of 50mM of 1.5mL, strong stirring 30min are added in thereto
Afterwards, by solution left standstill for a period of time, you can observe that solution is significantly layered.Supernatant liquor is shifted, it is molten to leave bottom pink colour
Liquid is ball-bar poly liquid solution.
Claims (5)
1. a kind of autoreduction preparation method of gold nano ball-bar polymer, it is characterised in that step is as follows：
(1) synthesis of seed liquor：
The three hydration tetra chlorauric acid solution of a concentration of 0.5mM of 2.5mL are placed in 20mL vials by (1a), are added in thereto
The cetyl trimethylammonium bromide solution of a concentration of 0.2M of 2.5mL, solution colour become yellowish-brown by colourless, obtain solution A；
A concentration of 0.01M sodium borohydride solutions of 0.3mL are diluted with water 0.5mL by (1b), are rapidly injected solution A, solution colour
Light brown is become from yellowish-brown immediately, and continues strong stirring 2min, obtains solution B；
(1c) by solution B under the conditions of 30 DEG C about 3 hours of aging to get seed liquor；
(2) synthesis of growth-promoting media：
0.617g enuatrols and 4.5g cetyl trimethylammonium bromides are placed in 500mL conical flasks by (2a), are added in thereto
The hot water that about 50 DEG C of 125mL.Stirring makes it naturally cool to 30 DEG C, obtains solution C；
(2b) adds in the silver nitrate solution of a concentration of 4mM of 9mL to solution C, stops stirring, it is made to stand 15min in 30 DEG C of constant temperature,
Obtain solution D；
(2c) adds in the three hydration tetra chlorauric acid solution of a concentration of 1mM of 125mL into solution D, stirs 90min, then adds
The hydrochloric acid stirring 15min of a concentration of 12.1M of 0.75mL, obtains solution E；
(2d) adds in the ascorbic acid solution of a concentration of 0.064mM of 0.625mL into solution E, and strong stirring 30s is to get growth
Liquid；
(3) synthesis of the gold nanorods of double base surfactant cladding：
(3a) takes 0.2mL seed liquors, is rapidly injected in growth-promoting media, strong stirring 30s；
(3b) stands aging 22h to get gold nanorods solution in 30 DEG C of constant temperature；
(4) acquisition of gold nanorods pure water solution：
The good gold nanorods solution of the aging obtained in (3b) is centrifuged 20min by (4a) under 9000rpm, sinks to gold nanorods
Centrifuge bottom of the tube；
(4b) is according to 1：1 volume ratio disperses centrifuge tube bottom precipitation in deionized water, to obtain gold nanorods pure water again
Solution；
(5) synthesis of ball-bar polymer：
(5a) takes the gold nanorods solution 3mL obtained in (4b), and it is a concentration of to add in 3mL thereto under conditions of strong stirring
10mM thiomalic acid aqueous solutions；
(5b) adds in sodium hydrate aqueous solution thereto, and solution ph is transferred to 9.5；
(5c) adds in the o-dichlorobenzene solution of a concentration of tetra- n-octyl ammonium bromides of 50mM of 1.5mL, strong stirring 30min thereto
Afterwards, by solution left standstill for a period of time, you can observe that solution is significantly layered.Supernatant liquor is shifted, it is molten to leave bottom pink colour
Liquid is ball-bar poly liquid solution.
2. a kind of autoreduction preparation method of gold nano ball-bar polymer according to claim 1, which is characterized in that by
1 abosrption spectrogram of attached drawing shows that longitudinal plasma resonance absorption peak of the gold nano ball-bar polymer is located near infrared region.
A kind of 3. autoreduction preparation method of gold nano ball-bar polymer according to claim 1, which is characterized in that step
Suddenly the gold nanorods prepared in (3b), a diameter of 12nm~18nm, length are 60nm~90nm.
A kind of 4. autoreduction preparation method of gold nano ball-bar polymer according to claim 1, which is characterized in that step
Suddenly the size of the gold nanosphere in the gold nano ball-bar polymer prepared in (5c) is 6~8nm.
A kind of 5. autoreduction preparation method of gold nano ball-bar polymer according to claim 1, which is characterized in that step
Suddenly the acquisition of gold nanorods pure water solution is according to 1 in (4b)：1 volume ratio divides the gold nanorods once centrifuged precipitation again
It dissipates in deionized water.
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Citations (8)
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| CN101343778A (en) * | 2008-08-29 | 2009-01-14 | 北京航空航天大学 | Process for producing golden nano stick with short length-diameter ratio |
| EP2156910A1 (en) * | 2008-08-20 | 2010-02-24 | Fujifilm Corporation | Composite metal nanorod, composite metal nanorod-containing composition, and polarization material |
| CN102367589A (en) * | 2011-09-15 | 2012-03-07 | 王利兵 | Preparation method of binary gold nanoparticle Janus assembly |
| CN102382816A (en) * | 2011-09-15 | 2012-03-21 | 王利兵 | Preparation method for chiral self-assembly material |
| US8257465B2 (en) * | 2008-03-03 | 2012-09-04 | University Of Washington | Crystalline noble metal nanostructures and methods for their preparation |
| CN102864493A (en) * | 2012-10-12 | 2013-01-09 | 江南大学 | Preparation method of gold nanorod chiral self-assembly material based on small organic molecule salts |
| CN104858445A (en) * | 2015-03-27 | 2015-08-26 | 南京邮电大学 | Controllable assembly method of plasmon polariton baseball 'corn' structure |
| CN107243629A (en) * | 2017-06-09 | 2017-10-13 | 山东博奥克生物科技有限公司 | A kind of new type structure of hud nano-particle and preparation method thereof |
-
2018
- 2018-01-10 CN CN201810022166.1A patent/CN108145176B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8257465B2 (en) * | 2008-03-03 | 2012-09-04 | University Of Washington | Crystalline noble metal nanostructures and methods for their preparation |
| EP2156910A1 (en) * | 2008-08-20 | 2010-02-24 | Fujifilm Corporation | Composite metal nanorod, composite metal nanorod-containing composition, and polarization material |
| CN101343778A (en) * | 2008-08-29 | 2009-01-14 | 北京航空航天大学 | Process for producing golden nano stick with short length-diameter ratio |
| CN102367589A (en) * | 2011-09-15 | 2012-03-07 | 王利兵 | Preparation method of binary gold nanoparticle Janus assembly |
| CN102382816A (en) * | 2011-09-15 | 2012-03-21 | 王利兵 | Preparation method for chiral self-assembly material |
| CN102864493A (en) * | 2012-10-12 | 2013-01-09 | 江南大学 | Preparation method of gold nanorod chiral self-assembly material based on small organic molecule salts |
| CN104858445A (en) * | 2015-03-27 | 2015-08-26 | 南京邮电大学 | Controllable assembly method of plasmon polariton baseball 'corn' structure |
| CN107243629A (en) * | 2017-06-09 | 2017-10-13 | 山东博奥克生物科技有限公司 | A kind of new type structure of hud nano-particle and preparation method thereof |
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