CN102699343A - Method for preparing gold nanoparticles - Google Patents
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- CN102699343A CN102699343A CN2012101381834A CN201210138183A CN102699343A CN 102699343 A CN102699343 A CN 102699343A CN 2012101381834 A CN2012101381834 A CN 2012101381834A CN 201210138183 A CN201210138183 A CN 201210138183A CN 102699343 A CN102699343 A CN 102699343A
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Abstract
The invention belongs to the field of a nano material and particularly relates to a method for preparing gold nanoparticles. The method selects 2,6-dipicolinic acid (PDCA) as a reducing agent to reduce chloroauric acid to generate the gold nanoparticles by reaction; and then the 2,6-dipicolinic acid is used as a protecting agent on the surfaces of the gold nanoparticles; and the reaction condition is moderate and the gold nanoparticles are spherical nanoparticles which are mono-dispersed and uniform. The obtained gold nanoparticles are characterized by an ultraviolet-visible light spectrum (UV-vis), a transmission electron microscope (TEM) and x-ray energy spectrum analysis. The result shows that the particles are spherical, are uniform in size, the diameters of the particles are 6-8nm and the dispersion degree of the gold nanoparticles is high. The method for preparing the gold nanoparticles has the advantages of convenience for operation, moderate condition, and high yield, adopts environment-friendly materials, and also can be used for controllably preparing the mono-dispersed gold nanoparticles.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related to a kind of method for preparing gold nano grain.
Background technology
In recent years; Noble metal nano particles (like the gold, silver nano particle) is because outstanding character such as its good optical, catalysis, bio-compatibilities; Receive researcher's extensive concern, the size of gold, silver nanoparticle, shape and structure control and corresponding property research become the forward position focus of material science and association area.Wherein gold nano grain is research a kind of nano material early, in biological study, generally is referred to as collaurum.Its particle size is generally between 1-100 nm; Because the character of surface plasma body resonant vibration; Variation with particle diameter presents various colors; Help perusal, have stronger colour developing ability, be widely used in numerous areas such as sensitization, catalysis, biological label, medical immunology, SERS.
The preparation method of gold nano grain mainly can be divided into physics method and chemical method; Wherein, commonly used is chemical method, and chemical method is that the compound (normally gold chloride) with gold is a raw material; Utilize the reproducibility reduction to generate golden nanometer particle; Reaction conditions such as amount through control temperature, reducing agent prepare particles of different sizes, and chemical method mainly comprises: aqueous phase oxidation reducing process, crystal seed method, phase transfer method etc.Wherein, the most classical Frens method [Mucic R C, Storhoff J J; Mirkin C A, Letsinger R L 1998, J. Am. Chem. Soc. 120 12674 – 12675.] be gold nano grain preparation method with the natrium citricum reduction; Can obtain the nanogold particle of 10-100 nm size range; Be to use the widest a kind of preparation method, the nanogold particle of the natrium citricum that obtains protection shows a monodisperse distribution; Particle surperficial electronegative, this method also can be used to prepare silver nano-grain.
Various in recent years preparation method of metal nanoparticles constantly develop, and people require to prepare the group that the method for gold nano grain modified pattern, size, the surface of the particle of preparation etc. can carry out controllable operating [Yang T, Li Z; Wang L; Guo CL, Sun YJ, Synthesis; Characterization; And Self-Assembly of Protein Lysozyme Monolayer-Stabilized Gold Nanoparticles [J]. Langmuir, 2007,23 (21): 10533 – 10538.].Yet most method obtains the nanometer of various patterns and size or structure, the pattern of micron has very big difference, even the pattern of nanogold particle and size are mostly inhomogeneous; And usually be accompanied by problem [Bri as R P such as separation difficulty; Hu M H, Qian L P, Lymar E S; Hainfeld J F; Gold Nanoparticle Size Controlled by Polymeric Au (I) Thiolate Precursor Size [J]. J. Am. Chem. Soc. 2008,130 (3): 975 – 982. Huanga K W, Yua C J; Tseng W L. Sensitivity enhancement in the colorimetric detection of lead (II) ion using gallic acid – capped gold nanoparticles:Improving size distribution and minimizing interparticle repulsion [J]. Biosensors and Bioelectronics; 2010,25 (5): 984 –, 989. Nadagouda M N, Hoag G; Collins J; Varma R S, Green Synthesis of Au Nanostructures at Room Temperature Using Biodegradable Plant Surfactants [J] .Cryst. Growth Des. 2009,9 (11): 4979 – 4983.].This its optical property of synthetic gold nano grain is not too obvious usually, can only be used to do catalyst etc. usually.Therefore, synthetic have regular morphology, and the method for the gold nano grain of size homogeneous has certain difficulty, and makes the gold nano grain stable in properties after synthesizing, and special groups is rich on the surface need select appropriate reductant and reaction condition especially.[Leontowich A F G, Calver C F, Dasog M; R W J Scott, Surface Properties of Water-Soluble Glycine-Cysteamine-Protected Gold Clusters [J] .Langmuir 2010,26 (2): 1285 – 1290. Serizawa T; Hirai Y, Aizawa M, Novel Synthetic Route to Peptide-Capped Gold Nanoparticles [J]. Langmuir 2009; 25 (20): 12229 –, 12234. Lin G H, Lu W S, Cui W J; Jiang L, A Simple Synthesis Method for Gold Nano-and Microplate Fabrication Using a Tree-Type Multiple-Amine Head Surfactant [J]. Cryst. Growth Des.2010,10 (3): 1118 – 1123.] and the gold nano grain of using in fields such as biological detection, biomedicines need have good optical character; Requirement granule-morphology rule; Size homogeneous, surface are prone to modify, and the preparation method is simple; Reaction condition is gentle; Can prepare in a large number, so, remain the hot subject of research in recent years for the method for preparing gold nano grain.
Summary of the invention
The purpose of this invention is to provide a kind of easy and simple to handle, mild condition, high, the material environment friendly of productive rate, and can controlledly prepare single method of disperseing gold nano grain again.
Often adopt the reduction gold chloride at present and prepare nanogold particle, the key that adopts this method to prepare gold nano grain is the selection of reducing agent, select appropriate reductant can guarantee to reduce preparation gold grain process not or have less multiple reaction to take place; Do not reproduce the generation of thing; Make the reaction raw materials gold chloride under the reduction of excessive slightly reducing agent, generate gold grain fully, do not have other product; The particle that obtains is under the protection of reducing agent, and size is even, good dispersion.The present invention selects 2, and dipicolimic acid 2 (PDCA) is as reducing agent, and the reaction of reduction gold chloride generates behind the gold nano grain on the gold nano grain surface as protective agent, and reaction condition is gentle, and the gold nano grain that obtains is monodispersed uniform spherical nano particle.Concrete method of operating is following:
2, dipicolimic acid 2 (PDCA) reduction gold chloride prepares gold nano grain:
At first with gold chloride (HAuCl
43H
2O) aqueous solution that in the darkroom, is made into 0.1M/L uses as stock solution, gets 2 of 20-50mL and 1-5M/L, and dipicolimic acid 2 aqueous solution 5-20mL mixes under the condition of water bath heating of 25-80 ° of C and stirs; Reaction continued after 15-30 minute, and the color of solution is red by original approaching colourless slowly pulverize, along with the increase color of time is deepened gradually; Become redness at last, after stopping to react, make solution slowly be cooled to room temperature; With centrifuge under the rotating speed that 5000-8000 changes centrifugal 10-15 minute, abandoning supernatant was removed unreacted reducing agent 2 with the solution of gained; Dipicolimic acid 2, the deposition of gained be ultrasonic again again be distributed to original isopyknic ultra-pure water in, just obtained 2; The gold nano grain of dipicolimic acid 2 protection is placed on refrigerator and cooled and hides preservation.
The gold nano grain that obtains characterizes through ultraviolet-visible spectrum (UV-vis), transmission electron microscope (TEM) and the analysis of x ray energy spectrum.The result shows; The ultraviolet-visible spectrum of gold nano grain (shown in accompanying drawing 1) has a characteristic absorption peak at the 518nm place, belong to the surface plasma body resonant vibration characteristic absorption for gold nano grain, and it is spherical having only a unimodal coating of particles that shows; The intensity of this absworption peak is higher; The productive rate that shows gold nano grain is higher, and peak position shows that the gold nano grain particle diameter is less between 515-525nm; The less gold nano grain good dispersion that shows of halfwidth possesses surface of good plasma resonance character.The transmission electron microscope of gold nano grain (shown in accompanying drawing 2) is the result show, particle is spherical, and size is even, and the diameter of particle is 6-8 nm, and the gold nano grain degree of scatter is high.X ray energy spectrum (EDX) analysis result (accompanying drawing 3) proves; Appearance among the figure characteristic peak of three kinds of elements, be respectively carbon, copper, gold, wherein the composition of copper source is copper mesh; Carbon then is the carbon film that comes from the copper mesh; And the composition of nano particle is a gold, therefore, the particle of proof preparation more intuitively be gold nano grain.
The present invention has following advantage:
1, preparation method provided by the invention is simple, quick, easy to operate.
2, size of nanometer gold grain homogeneous, the good dispersion of preparation possess surface of good plasma resonance character.
3, the present invention is prone to preparation and preserves; Under 4 ° of C conditions, can preserve 10～15 months.
4, agents useful for same of the present invention and operating process all have no side effect.
Description of drawings
The uv-visible absorption spectra of accompanying drawing 1, gold nano grain
The transmission electron microscope figure of accompanying drawing 2, gold nano grain
The EDX of accompanying drawing 3, gold nano grain (analysis of x ray energy spectrum) elementary analysis spectrogram
The specific embodiment
Embodiment 1:
At first in the darkroom with gold chloride (HAuCl
43H
2O) be made into the aqueous solution of 0.1M/L, get 2 of 20mL and 5M/L, dipicolimic acid 2 aqueous solution 20mL mixes under the condition of water bath heating of 80 ° of C and stirs; Reaction continued after 15 minutes, and the color of solution is red by original approaching colourless slowly pulverize, along with the increase color of time is deepened gradually; Become redness at last, after stopping to react, make solution slowly be cooled to room temperature; With centrifuge under 8000 rotating speeds that change centrifugal 10 minutes, abandoning supernatant was removed unreacted reducing agent 2 with the solution of gained; Dipicolimic acid 2; The deposition of gained is ultrasonic again again be distributed to original isopyknic ultra-pure water in, just obtained 2, the gold nano grain of dipicolimic acid 2 protection.The gold nano grain that obtains is tested its absorption through ultraviolet-visible spectrum (UV-vis), verify its surface plasma body resonant vibration character, then gold nano grain solution is placed on refrigerator and cooled and hides preservation.
Embodiment 2:
At first in the darkroom with gold chloride (HAuCl
43H
2O) be made into the aqueous solution of 0.1M/L, get 2 of 30mL and 5M/L, dipicolimic acid 2 aqueous solution 5mL mixes under the condition of water bath heating of 50 ° of C and stirs; Reaction continued after 30 minutes, and the color of solution is red by original approaching colourless slowly pulverize, along with the increase color of time is deepened gradually; Become redness at last, after stopping to react, make solution slowly be cooled to room temperature; With centrifuge under 6000 rotating speeds that change centrifugal 15 minutes, abandoning supernatant was removed unreacted reducing agent 2 with the solution of gained; Dipicolimic acid 2; The deposition of gained is ultrasonic again again be distributed to original isopyknic ultra-pure water in, just obtained 2, the gold nano grain of dipicolimic acid 2 protection.The gold nano grain that obtains is tested its absorption through ultraviolet-visible spectrum (UV-vis), verify its surface plasma body resonant vibration character, gold nano grain solution is placed in the refrigerator of 4 ° of C preserves then.
Embodiment 3:
At first in the darkroom with gold chloride (HAuCl
43H
2O) be made into the aqueous solution of 0.1M/L, get 2 of 25mL and 5M/L, dipicolimic acid 2 aqueous solution 15mL mixes under the condition of water bath heating of 70 ° of C and stirs; Reaction continued after 20 minutes, and the color of solution is red by original approaching colourless slowly pulverize, along with the increase color of time is deepened gradually; Become redness at last, after stopping to react, make solution slowly be cooled to room temperature; With centrifuge under 7000 rotating speeds that change centrifugal 15 minutes, abandoning supernatant was removed unreacted reducing agent 2 with the solution of gained; Dipicolimic acid 2; The deposition of gained is ultrasonic again again be distributed to original isopyknic ultra-pure water in, just obtained 2, the gold nano grain of dipicolimic acid 2 protection.The gold nano grain that obtains is tested its absorption through ultraviolet-visible spectrum (UV-vis), verify its surface plasma body resonant vibration character, gold nano grain solution is placed in the storage bin of 4 ° of C preserves then.
Claims (3)
1. a method for preparing gold nano grain is characterized in that at first with gold chloride HAuCl
43H
2O is made into 0.1M/L in the darkroom the aqueous solution uses as stock solution, gets 2 of 20-50mL and 1-5M/L, and dipicolimic acid 2 aqueous solution 5-20mL mixes under the condition of water bath heating of 25-80 ° of C and stirs; Reaction continued after 15-30 minute, and the color of solution is red by original approaching colourless slowly pulverize, along with the increase color of time is deepened gradually; Become redness at last, after stopping to react, make solution slowly be cooled to room temperature; With centrifuge under the rotating speed that 5000-8000 changes centrifugal 10-15 minute, abandoning supernatant was removed unreacted reducing agent 2 with the solution of gained; Dipicolimic acid 2, the deposition of gained be ultrasonic again again be distributed to original isopyknic ultra-pure water in, just obtained 2; The gold nano grain of dipicolimic acid 2 protection is placed on refrigerator and cooled and hides preservation.
2. according to the described method of claim 1; It is characterized in that under the condition of water bath heating of 70 ° of C, mixing and stirring; Reaction continues 20 minutes, and the solution of gained is preserved in the centrifugal storage bin that gold nano grain solution was placed in 15 minutes 4 ° of C under the rotating speed of 7000 commentaries on classics with centrifuge.
3. the gold nano grain for preparing according to the described method of claim 1.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103808717A (en) * | 2014-02-14 | 2014-05-21 | 哈尔滨师范大学 | Method for detecting mercury ions by adopting colorimetric method |
| CN103852467A (en) * | 2014-03-13 | 2014-06-11 | 哈尔滨师范大学 | Chromium ion colorimetric detection probe and application method thereof |
| CN104070179A (en) * | 2014-07-21 | 2014-10-01 | 山西农业大学 | Method for preparing nanogold through mango peel reducing agent |
| CN104308174A (en) * | 2014-09-25 | 2015-01-28 | 中国科学院化学研究所 | Method for dispersing and/or purifying gold nano-sheets |
| CN104690265A (en) * | 2015-03-17 | 2015-06-10 | 福州大学 | Golden nanostars and preparation method and application thereof |
| CN106290182A (en) * | 2016-07-18 | 2017-01-04 | 西安交通大学 | The simple and easy method of a kind of gold nanorods self assembly and the application in mercury ion detecting thereof |
| CN106936059A (en) * | 2017-04-06 | 2017-07-07 | 上海大学 | Transmitting organic laser thin-film device with the enhanced optical pumping face of gold nano grain, using and preparation method thereof |
| US10099191B1 (en) | 2017-06-22 | 2018-10-16 | Tripod Technology Corporation | Method of making colloidal metal nanoparticles |
| DE102017116090A1 (en) * | 2017-06-19 | 2018-12-20 | Tripod Technology Corporation | Process for the preparation of colloidal metal nanoparticles |
| CN110449595A (en) * | 2019-07-11 | 2019-11-15 | 四川大学 | The method and hydrophobicity gold, silver nano particle of step preparation hydrophobicity gold, silver nano particle in a kind of aqueous solution |
| CN113433110A (en) * | 2021-06-22 | 2021-09-24 | 西安邮电大学 | Preparation method for generating substrate with honeysuckle dendritic crystal flower-like nano structure by in-situ substitution method |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103808717A (en) * | 2014-02-14 | 2014-05-21 | 哈尔滨师范大学 | Method for detecting mercury ions by adopting colorimetric method |
| CN103852467A (en) * | 2014-03-13 | 2014-06-11 | 哈尔滨师范大学 | Chromium ion colorimetric detection probe and application method thereof |
| CN103852467B (en) * | 2014-03-13 | 2016-06-29 | 哈尔滨师范大学 | A kind of chromium ion colorimetric detection probes and application process thereof |
| CN104070179A (en) * | 2014-07-21 | 2014-10-01 | 山西农业大学 | Method for preparing nanogold through mango peel reducing agent |
| CN104308174A (en) * | 2014-09-25 | 2015-01-28 | 中国科学院化学研究所 | Method for dispersing and/or purifying gold nano-sheets |
| CN104690265B (en) * | 2015-03-17 | 2017-05-10 | 福州大学 | Golden nanostars and preparation method and application thereof |
| CN104690265A (en) * | 2015-03-17 | 2015-06-10 | 福州大学 | Golden nanostars and preparation method and application thereof |
| CN106290182A (en) * | 2016-07-18 | 2017-01-04 | 西安交通大学 | The simple and easy method of a kind of gold nanorods self assembly and the application in mercury ion detecting thereof |
| CN106936059A (en) * | 2017-04-06 | 2017-07-07 | 上海大学 | Transmitting organic laser thin-film device with the enhanced optical pumping face of gold nano grain, using and preparation method thereof |
| DE102017116090A1 (en) * | 2017-06-19 | 2018-12-20 | Tripod Technology Corporation | Process for the preparation of colloidal metal nanoparticles |
| AU2018201824B2 (en) * | 2017-06-19 | 2019-11-14 | Tripod Technology Corporation | Method of making colloidal metal nanoparticles |
| DE102017116090B4 (en) * | 2017-06-19 | 2021-06-10 | Tripod Technology Corporation | Process for the production of colloidal metal nanoparticles |
| US10099191B1 (en) | 2017-06-22 | 2018-10-16 | Tripod Technology Corporation | Method of making colloidal metal nanoparticles |
| CN110449595A (en) * | 2019-07-11 | 2019-11-15 | 四川大学 | The method and hydrophobicity gold, silver nano particle of step preparation hydrophobicity gold, silver nano particle in a kind of aqueous solution |
| CN113433110A (en) * | 2021-06-22 | 2021-09-24 | 西安邮电大学 | Preparation method for generating substrate with honeysuckle dendritic crystal flower-like nano structure by in-situ substitution method |
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Application publication date: 20121003 |