CN105965029B - The synthetic method of water-soluble monodispersed spherical gold-silver alloy nano particle - Google Patents
The synthetic method of water-soluble monodispersed spherical gold-silver alloy nano particle Download PDFInfo
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- CN105965029B CN105965029B CN201610387543.2A CN201610387543A CN105965029B CN 105965029 B CN105965029 B CN 105965029B CN 201610387543 A CN201610387543 A CN 201610387543A CN 105965029 B CN105965029 B CN 105965029B
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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
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- 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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- 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
Abstract
The present invention relates to the synthetic method of water-soluble monodispersed spherical gold-silver alloy nano particle, sodium citrate, gold chloride, silver nitrate and ferrous sulfate are configured to solution respectively first by ultra-pure water;Then by volume 40:7:1‑20:0.88 17.5 weigh sodium citrate solution (two parts), chlorauric acid solution, silver nitrate solution and copperas solution respectively, and chlorauric acid solution is added in boiling water;A sodium citrate solution and copperas solution are added in the boiling water containing gold chloride successively, after another sodium citrate solution and silver nitrate solution are mixed into 37 minutes, are rapidly added in the mixed liquor of boiling;Boiling is finally kept, room temperature is cooled to after being heated to reflux 1 hour, that is, obtains water-soluble monodispersed spherical gold-silver alloy nano particle.The present invention is simple to operate, the high quality component size adjustable that can obtain, water solubility, single dispersing, spherical gold-silver alloy nano particle.
Description
Technical field
It is used to synthesize component size adjustable, water solubility, single dispersing, spherical electrum nanometer the present invention relates to one kind
The method of grain, it is homogeneous to prepare specifically to reduce gold chloride and silver nitrate simultaneously using the sodium citrate of ferrous ion auxiliary
Gold-silver alloy nano particle method, belong to noble metal nano particles synthesis technical field.
Background technology
The noble metal granule size such as gold, silver is small to can show many special photoelectric properties, such as table during Nano grade
Face plasma resonance effect etc..And these performances are strongly depend on pattern, size and the component of nano particle.Gold silver nanometer particle
Based on its excellent surface plasma resonance effect, the prospect of being widely applied is illustrated in surface Raman enhancement test, is improved
Detection sensitivity, realize liquid detecting and Single Molecule Detection etc..For other metals, silver is because of the light of its protrusion
The Electromagnetic enhancement of performance and visible region is learned, is widely applied in the surface Raman enhancement test in the fields such as chemistry and biology;
But because its chemical stability is bad, detection in many adverse circumstances (such as strong acid, highly basic, oxide) substantially by
Limitation.In contrast, gold nano grain has excellent chemical stability, corrosion resistance and oxidation resistent susceptibility.Therefore design
Gold-silver alloy nano particle is synthesized, it is had the chemically stable of the excellent optical property of silver nano-grain and gold nano grain concurrently
Property, more it is widely applied with realizing.
In the past more than ten years, the preparation on gold-silver alloy nano particle has many people to do substantial amounts of research, bag
Include ultrasonic method, laser ablation method, photocatalytic method, chemical reduction method etc..But in the side of countless synthesis gold-silver alloy nano particles
In method, only high temperature or multistep processes can just obtain the adjustable gold-silver alloy nano particle of size small range at present, and uncomfortable
For producing in enormous quantities.Cut-off is up to the present, a wide range of by simple experiment condition and step 1 step synthesis component size
Adjustable gold-silver alloy nano particle is still a great problem.In addition, the part on gold-silver alloy nano particle surface is to its surface
Raman-enhancing to have a great impact, poisonous organic ligand can cause powerful interference to test, and be unfavorable for them in life
Application in the fields such as thing medical science.Sodium citrate is a kind of biocompatibility part, is easily replaced by other biomolecule, antibody etc.
Change, and surface Raman enhancement will not be tested and had any impact, so, the stable electrum nanometer of sodium citrate part
Particle has vast application prospect.
At present, in the various methods of gold-silver alloy nano particle are prepared as part using sodium citrate, due to Jin Heyin's
Growth rate is different, and obtained product is often the mixing production of component, pattern and the inhomogenous gold-silver alloy nano particle of size
Thing.Therefore, the weak part of one-step synthesis method, a wide range of adjustable and size uniformity the water-soluble monodispersed gold of component size are passed through
Silver alloy nano particle is a no small challenge.The solution of these problems can certainly widen electrum nanometer significantly
Application of the particle in biomedical detection, sensor and surface Raman enhancement etc..
The content of the invention
The present invention is for deficiency existing for existing preparation gold-silver alloy nano particle technology, there is provided it is a kind of it is simple to operate,
Synthesize the synthetic method of efficiently water-soluble monodispersed spherical gold-silver alloy nano particle.
The synthetic method of the water-soluble monodispersed spherical gold-silver alloy nano particle of the present invention, comprises the following steps:
(1) using ultra-pure water by required raw material sodium citrate (reducing agent, stabilizer), gold chloride (soluble precursor),
Silver nitrate (soluble silver salt) and ferrous sulfate (auxiliary additive) are configured to the citric acid that mass percent concentration is 1% respectively
Silver nitrate solution that chlorauric acid solution that sodium solution, mass percent concentration are 1%, mass percent concentration are 1% and mole
Concentration is 0.5 mM/l of copperas solution;
(2) by volume 40:7:1-20:0.88-17.5 ratio measure respectively sodium citrate solution, chlorauric acid solution,
Silver nitrate solution and copperas solution, wherein sodium citrate solution weigh two parts by same ratio;
(3) by chlorauric acid solution and ultra-pure water 1:537.14-560 volume ratio chlorauric acid solution is added in boiling water;
(4) a sodium citrate solution and copperas solution are sequentially added in the boiling water containing gold chloride, turns into boiling
Rise mixed liquor;
(5) by another sodium citrate solution and after silver nitrate solution mixing 3-7 minutes, it is rapidly added boiling mixed liquor
In;
(6) boiling is kept, room temperature is cooled to after being heated to reflux 1 hour, that is, obtains water-soluble mono and disperses spherical gold and silver conjunction
Gold nano grain.
The present invention using ferrous ion aid in reduction of sodium citrate gold chloride and silver nitrate come prepare component size adjustable,
Water solubility, single dispersing, spherical gold-silver alloy nano particle, compared to more other synthetic methods, this method is simple to operate, can
High quality, component size adjustable, water solubility, monodispersed spherical electrum that other existing methods can not obtain is obtained to receive
Rice grain.
Brief description of the drawings
Fig. 1 is the transmission electron microscope for the water-soluble monodispersed spherical gold-silver alloy nano particle that the present invention synthesizes
Photo.
Wherein:(a)-(h) is respectively embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, reality
Apply the particle diameter that example 7 and embodiment 8 obtain be respectively 10 nanometers, 11 nanometers, 16 nanometers, 25 nanometers, 30 nanometers, 46 nanometers, 64 receive
The transmission electron microscope photo of rice and 80 nanometers of water-soluble monodispersed spherical gold-silver alloy nano particle.
Embodiment
Embodiment 1
It is small that glassware used (twoport flask and 5 milliliters of serum bottle) is put into immersion 2 in the chloroazotic acid newly configured first
Shi Hou, cleaned, be dried for standby with sodium nitrate saturated solution and ultra-pure water.
Required raw material sodium citrate, gold chloride, silver nitrate and ferrous sulfate are each configured to solution using ultra-pure water, its
The mass percent concentration of middle sodium citrate solution is 1%, and the mass percent concentration of chlorauric acid solution is 1%, and silver nitrate is molten
The mass percent concentration of liquid is 1%, and the molar concentration of copperas solution is 0.5 mM/l.
By volume 40:7:1:17.5 ratio weighs 0.5 milliliter of sodium citrate solution (two parts), chlorauric acid solution respectively
218.8 microlitres of 87.5 microlitres, 12.5 microlitres of silver nitrate solution and copperas solution.
Twoport flask is fixed on warm table and adds ultra-pure water (chlorauric acid solution and the ultrapure water body of 47-49 milliliters
Product is than being 1:537.14-560), it is heated rapidly to 100 degrees Celsius of backflows;87.5 microlitres of chlorauric acid solution is added in boiling water;
Then 0.5 milliliter of sodium citrate solution and 218.8 microlitres of copperas solutions are added in the boiling water containing gold chloride successively;Will
0.5 milliliter of sodium citrate solution and after 12.5 microlitres of silver nitrate solution mixing 3-7 minutes, is rapidly added in the mixed liquor of boiling;
Ensure that it is 50 milliliters to react cumulative volume, keeps boiling, after being heated to reflux 1 hour, is cooled to room temperature, you can obtains particle diameter and received for 10
The water-soluble monodispersed spherical gold-silver alloy nano particle of rice.
The transmission electron microscope photo such as Fig. 1 for the water-soluble monodispersed spherical gold-silver alloy nano particle that the present embodiment obtains
In shown in (a).
Embodiment 2
The present embodiment difference from Example 1 is that the dosage of silver nitrate solution is 25 microlitres, makes sodium citrate solution, chlorine
The volume ratio of auric acid solution, silver nitrate solution and copperas solution is 40:7:2:17.5 (0.5 milliliter, 87.5 microlitres, it is 25 micro-
Rise and 218.8 microlitres).
Remaining condition is same as Example 1, can obtain the monodispersed spherical electrum of the nano-water soluble of particle diameter 11
In nano particle, its transmission electron microscope photo such as Fig. 1 shown in (b).
Embodiment 3
The present embodiment difference from Example 1 is that the dosage of silver nitrate is 50 microlitres, makes sodium citrate solution, gold chloride
The volume ratio of solution, silver nitrate solution and copperas solution is 40:7:4:17.5 (0.5 milliliter, 87.5 microlitres, 50 microlitres and
218.8 microlitres).
Remaining condition is same as Example 1, and the water-soluble monodispersed spherical gold and silver that can obtain 16 nanometers of particle diameter closes
Gold nano grain, shown in its transmission electron microscope photo such as Fig. 1 (c).
Embodiment 4
The present embodiment difference from Example 1 one is that the dosage of silver nitrate is 50 microlitres, second, copperas solution
Dosage is 65.7 microlitres, and the volume ratio for making sodium citrate solution, chlorauric acid solution, silver nitrate solution and copperas solution is
40:7:4:5.26 (0.5 milliliters, 87.5 microlitres, 50 microlitres and 65.7 microlitres).
Remaining condition is same as Example 1, and the water-soluble monodispersed spherical gold and silver that can obtain 25 nanometers of particle diameter closes
Gold nano grain, shown in its transmission electron microscope photo such as Fig. 1 (d).
Embodiment 5
The present embodiment difference from Example 1 one is that the dosage of silver nitrate is 50 microlitres, second, copperas solution
Dosage is 43.8 microlitres, and the volume ratio for making sodium citrate solution, chlorauric acid solution, silver nitrate solution and copperas solution is
40:7:4:3.5 (0.5 milliliters, 87.5 microlitres, 50 microlitres and 43.8 microlitres).
Remaining condition is same as Example 1, and the water-soluble monodispersed spherical gold and silver that can obtain 30 nanometers of particle diameter closes
Gold nano grain, shown in its transmission electron microscope photo such as Fig. 1 (e).
Embodiment 6
The present embodiment difference from Example 1 one is that the dosage of silver nitrate is 250 microlitres, second, copperas solution
Dosage is 43.8 microlitres, and the volume ratio for making sodium citrate solution, chlorauric acid solution, silver nitrate solution and copperas solution is
40:7:20:3.5 (0.5 milliliters, 87.5 microlitres, 250 microlitres and 43.8 microlitres).
Remaining condition is same as Example 1, and the water-soluble monodispersed spherical gold and silver that can obtain 46 nanometers of particle diameter closes
Gold nano grain, shown in its transmission electron microscope photo such as Fig. 1 (f).
Embodiment 7
The present embodiment difference from Example 1 one is that the dosage of silver nitrate is 250 microlitres, second, copperas solution
Dosage is 21.9 microlitres, and the volume ratio for making sodium citrate solution, chlorauric acid solution, silver nitrate solution and copperas solution is
40:7:20:1.75 (0.5 milliliters, 87.5 microlitres, 250 microlitres and 21.9 microlitres).
Remaining condition is same as Example 1, and the water-soluble monodispersed spherical gold and silver that can obtain 64 nanometers of particle diameter closes
Gold nano grain, shown in its transmission electron microscope photo such as Fig. 1 (g).
Embodiment 8
The present embodiment difference from Example 1 one is that the dosage of silver nitrate is 250 microlitres, second, copperas solution
Dosage is 10.9 microlitres, and the volume ratio for making sodium citrate solution, chlorauric acid solution, silver nitrate solution and copperas solution is
40:7:20:0.88 (0.5 milliliter, 87.5 microlitres, 250 microlitres and 10.9 microlitres).
Remaining condition is same as Example 1, and the water-soluble monodispersed spherical gold and silver that can obtain 80 nanometers of particle diameter closes
Gold nano grain, shown in its transmission electron microscope photo such as Fig. 1 (h).
Claims (1)
1. a kind of synthetic method of the monodispersed spherical gold-silver alloy nano particle of water solubility, it is characterized in that:Including following step
Suddenly:
(1) required raw material sodium citrate, gold chloride, silver nitrate and ferrous sulfate are configured to quality percentage respectively using ultra-pure water
Chlorauric acid solution that sodium citrate solution that specific concentration is 1%, mass percent concentration are 1%, mass percent concentration 1%
Silver nitrate solution and molar concentration be 0.5 mM/l of copperas solution;
(2) by volume 40:7:1-20:0.88-17.5 ratio measures sodium citrate solution, chlorauric acid solution, nitric acid respectively
Silver-colored solution and copperas solution, wherein sodium citrate solution weigh two parts by same ratio;
(3) by chlorauric acid solution and ultra-pure water 1:537.14-560 volume ratio chlorauric acid solution is added in boiling water;
(4) a sodium citrate solution and copperas solution are sequentially added in the boiling water containing gold chloride, it is mixed turns into boiling
Close liquid;
(5) by another sodium citrate solution and after silver nitrate solution mixing 3-7 minutes, it is rapidly added in boiling mixed liquor;
(6) boiling is kept, room temperature is cooled to after being heated to reflux 1 hour, that is, obtains water-soluble mono and disperses spherical electrum and receive
Rice grain.
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JP2006045655A (en) * | 2004-08-09 | 2006-02-16 | Mitsubishi Materials Corp | Silver nanoparticle and production method therefor |
CN101312800A (en) * | 2005-12-08 | 2008-11-26 | 住友金属矿山株式会社 | Liquid colloidal dispersion of silver particles, coating liquid for forming silver film, manufacturing method and silver film |
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