CN106623964A - Preparing method of tree-like structure silver nanometer particles - Google Patents
Preparing method of tree-like structure silver nanometer particles Download PDFInfo
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- CN106623964A CN106623964A CN201610821438.5A CN201610821438A CN106623964A CN 106623964 A CN106623964 A CN 106623964A CN 201610821438 A CN201610821438 A CN 201610821438A CN 106623964 A CN106623964 A CN 106623964A
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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
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Abstract
The invention discloses an environment-friendly synthetic method for novel tree-like structure silver nanometer particles. According to the method, on the condition without existence of templates, cysteine or glutathione is utilized as a reducing agent and a capping agent, and the tree-like structure silver nanometer particles are prepared and obtained easily and fast. The method is mild in reaction condition, easy and convenient to operate and small in environmental pollution, and provides a simple idea for preparing the anisotropic nanometer particles. According to the basic scheme, the method comprises the following steps that 1, the reducing agent and silver-containing metal salt are weighed; 2, the metal salt weighed in the step 1 is dissolved in distilled water to prepare a metal saline solution, and the reducing agent is dissolved in the distilled water; and 3, the metal saline solution in the step 2 and a reducing agent solution are mixed according to the molar ratio being (1-5):5, the pH value is adjusted to be 6-7, and the mixture is stirred and reacts in a thermostat water bath for a period of time to obtain the particles.
Description
Technical field
The present invention relates to the technical field of nano material, and in particular to a kind of preparation of novel tree-like structure Nano silver grain
Method.
Background technology
Nano material refer in three dimensions it is at least one-dimensional in nanoscale scope (usually 1～100nm)
Grain or the material being made up of as elementary cell them.Nano particle can be divided three classes substantially：(1) zero dimension, refers to three dimensions
Yardstick is in nanoscale, such as spherical nanoparticle；(2) it is one-dimensional, refer to that there is bidimensional in space in nanoscale, such as nano wire
(line), nanometer rods (bar), nanotube etc.；(3) two dimension, refer to have in three dimensions it is one-dimensional in nanoscale, wherein just including nanometer
Piece, nano thin-film etc..In in the past few decades, people have synthesized the noble metal nano grain of different-shape using various methods
Son, systematically have studied physics, chemistry and the optical characteristics of noble metal nano particles, explore the microcosmic life of metal nanoparticle
Long mechanism, develops them in catalysis, photonic propulsion, plasma optics, optical sensing, biomarker, medical imaging, Yi Jibiao
Face strengthens all many function and applications such as Raman spectrum, achieves many important progress, also becomes this field and grinds
Study carefully focus.
Tree nano-particle is a kind of nano-particle assembling knot for passing through ordered fabrication by single nano-particle
Structure, is that single nano-particle passes through to align, and forms dendritic structure.Its more traditional decentralized nano-particle has richer
The optical characteristics and electronics property of richness, has a wide range of applications in the nano-devices such as manufacture electronics, photoelectron and sensor
Prospect.The synthesis of traditional tree metal nanoparticle is nearly all based on template assemblies, however, no matter molten
The ligand molecular soft template of offer identification or interaction used in liquid, or the hard template based on the surface of solids,
Necessary to being all metal nanoparticle space structure assembling process, but there is chemical reagent pollution in template, and reactions steps are numerous
The defect such as trivial, its product is difficult to large-scale practical application, also restrained in biomedicine field application.
For above-mentioned deficiency, it is an object of the invention to provide one kind without template under conditions of existing, using half Guang
, used as reducing agent and activating agent, a step obtains tree Nano silver grain for propylhomoserin or reductive glutathione.The method is reacted
Mild condition, easy to operate, environmental pollution is little, has important using value in modern science field.
The content of the invention
The invention discloses a kind of green synthesis method of novel tree-like structure Nano silver grain, it is desirable to provide one kind is not having
Under conditions of with the presence of template, by the use of cysteine (L-cys) or reductive glutathione as reducing agent and agent of attaching the names of pre-determined candidates, simply
Tree Nano silver grain is rapidly prepared, the method reaction condition is gentle, and easy to operate, environmental pollution is little, is system
Standby anisotropic nano-particle provides simple thinking.
The preparation method of tree Nano silver grain of the present invention, comprises the steps：
1) reducing agent and argentiferous slaine are weighed respectively；
2) by step 1) dissolving metal salts that weigh prepare metal salt solution, and reducing agent dissolves in distilled water；
3) by step 2) in reductant solution and metal salt solution in molar ratio 1～5:5 mixing, adjust pH value 6-7,70
Stirring reaction 4h in DEG C thermostat water bath, obtains final product.
The environment-friendly preparation method thereof of above-mentioned tree Nano silver grain, described metal salt solution is dissolved in steaming for silver nitrate
One of silver nitrate aqueous solution that distilled water is obtained or silver ammino solution；Described reducing agent is cysteine or reproducibility
One of glutathione；When adjusting pH value conditioning agent used be NaOH either potassium hydroxide or ammoniacal liquor wherein it
One.
During the present invention prepares tree Nano silver grain, studying for a long period of time by inventor is set
Material molar ratio and reaction condition prepared by shape structure Nano silver grain, reducing agent is tied with the mol ratio of silver ion to synthesizing tree-like
The Nano silver grain of structure is most important；The control of reaction condition such as temperature, pH and whipping process etc. is whether there is, to tree
The formation of nano-particle can produce significantly impact.Add the amount of L-cys different in mixed system, the Nano silver grain of synthesis
Size and pattern also difference.By the mol ratio for changing L-cys and silver nitrate, silver nanoparticle of different shapes can be obtained
Particle.The mol ratio of L-cys/Ag+ is less than 3:When 5, the presence that Electronic Speculum collection of illustrative plates does not show nano-particle is observed；Work as L-cys/Ag
+ mol ratio be 4:When 5, the silver nano-grain for obtaining is presented spherical or spherical mostly, is gone back without enough silver atoms
Original out forms dendritic structure；When the mol ratio with L-cys/Ag+ gradually increases to 5:5, nano-particle now is presented
Dendroid.
Compared with prior art, the present invention provide technical scheme without template exist under conditions of, using half Guang ammonia
Acid or reductive glutathione make reducing agent and agent of attaching the names of pre-determined candidates, and tree Nano silver grain is prepared under heating environment, react
Mild condition, environmental friendliness is easy to operate, energy saving.It is reported that, easy fresh breeze, Tae Gwan Park et al. are also prepared for tree
Shape structure Nano silver grain, and the pattern of this research is closer to dendroid.
Tree Nano silver grain prepared by the present invention is coated by the oxidation product of cysteine, is effectively increased
The stability and biocompatibility of nano-particle, compares with metal nanoparticle with reguline metal, there is the light of more horn of plenty
Characteristic and electronics property are learned, particularly when the nano-devices such as electronics, photoelectron and sensor are manufactured, widely should be had
With；Also it is capable of achieving the large-scale application of metal nanoparticle biologic medical detection field.
Description of the drawings
Fig. 1 is the TEM image of the tree Nano silver grain prepared by embodiment 1；
Fig. 2 is the HR-TEM images of the tree Nano silver grain prepared by embodiment 1；
Specific embodiment
For a better understanding of the present invention, with reference to specific embodiment, the present invention is expanded on further.It should be understood that following
Embodiment only illustrates the present invention, rather than for limiting the scope of the invention.NM experimental technique in embodiment, generally according to
Conventional method is operated.
Embodiment 1
121mg cysteines are accurately weighed, in being dissolved in 100ml distilled water solutions, the half Guang ammonia of 10mmol/L is configured to
Acid solution, accurately weighs 170mg silver nitrates, and with 100ml water dissolves are distilled, and is configured to the silver nitrate solution of 10mmol/L.
To 5mL under the conditions of temperature T=70 DEG C and pH=6.5,5ml is added in the silver nitrate solution of 10mmol/L,
The cysteine solution of 10mmol/L, thorough stirring reaction 4h is finally obtained the nanoparticles solution of brown color, and constant volume
To 10mL.In course of reaction device is whisked come controlling reaction temperature with constant temperature magnetic force.
Embodiment 2
307.3mg reductive glutathiones are accurately weighed, in being dissolved in 100ml distilled water solutions, 10mmol/L is configured to
Reductive glutathione solution, accurately weigh 170mg silver nitrates, with 100ml distill water dissolves, be configured to the nitre of 10mmol/L
Sour silver solution.
To 5mL under the conditions of temperature T=70 DEG C and pH=6.5,2ml is added in the silver nitrate solution of 10mmol/L,
The reductive glutathione solution of 10mmol/L, thorough stirring reaction 4h is finally obtained the nanoparticles solution of brown color,
And it is settled to 10mL.In course of reaction device is whisked come controlling reaction temperature with constant temperature magnetic force.
Embodiment 3
121mg cysteines are accurately weighed, in being dissolved in 100ml distilled water solutions, the half Guang ammonia of 10mmol/L is configured to
Acid solution, accurately weighs 170mg silver nitrates, uses 10%100ml ammonia solvents, is configured to the silver ammino solution of 10mmol/L.
To 5mL under the conditions of temperature T=70 DEG C and pH=6.5,5ml, 10mmol/ are added in the silver ammino solution of 10mmol/L
The cysteine solution of L, thorough stirring reaction 4h is finally obtained the nanoparticles solution of brown color, and is settled to 10mL.
In course of reaction device is whisked come controlling reaction temperature with constant temperature magnetic force.
Embodiment 4
307.3mg reductive glutathiones are accurately weighed, in being dissolved in 100ml distilled water solutions, 10mmol/L is configured to
Reductive glutathione solution, accurately weigh 170mg silver nitrates, use 10%100ml ammonia solvents, be configured to 10mmol/L's
Silver ammino solution.
To 5mL under the conditions of temperature T=70 DEG C and pH=6.5,3ml, 10mmol/ are added in the silver ammino solution of 10mmol/L
The reductive glutathione solution of L, thorough stirring reaction 4h is finally obtained the nanoparticles solution of brown color, and constant volume
To 10mL.In course of reaction device is whisked come controlling reaction temperature with constant temperature magnetic force.
The present invention adopts cysteine green syt tree Nano silver grain, whole process not to use any adjuvant
And derivant, prepared tree Nano silver grain coated by the oxidation product of cysteine, effectively increases nanometer
The stability and biocompatibility of particle.Now by taking tree Nano silver grain prepared in embodiment 1 as an example, with reference to attached
Fig. 1-2 is described.The TEM image of tree Nano silver grain can be seen that the Yin Na synthesized by cysteine from Fig. 1
Rice corpuscles presents obvious tree；From Fig. 2 HR-TEM images, it can be seen that constitute the nano grain of silver sublist of dendritic morphology
Face is coated by layer of substance, and Jing infared spectrum validating analysis are cysteine or its oxidation product, play stabilization.It is right above
The specific embodiment of the present invention is described.It is to be appreciated that above-mentioned particular implementation is the invention is not limited in, this
Art personnel can within the scope of the claims make various modifications or modification, and this is had no effect in the essence of the present invention
Hold.
Claims (4)
1. a kind of preparation method of tree Nano silver grain, it is characterised in that comprise the following steps：
1) reducing agent and argentiferous slaine are weighed respectively；
2) by step 1) dissolving metal salts that weigh prepare metal salt solution, and reducing agent dissolves in distilled water；
3) by step 2) in reductant solution and metal salt solution in molar ratio 1～5:5 mixing, adjust pH value 6-7, in 70 DEG C of perseverances
Stirring reaction 4h in warm water bath, obtains final product.
2. a kind of preparation method of tree Nano silver grain as claimed in claim 1, it is characterised in that described metal
Salting liquid is dissolved in one of silver nitrate aqueous solution or silver ammino solution that distilled water obtains for silver nitrate.
3. a kind of preparation method of tree Nano silver grain as claimed in claim 1 or 2, it is characterised in that described
Reducing agent is one of cysteine or reductive glutathione.
4. the preparation method of a kind of tree Nano silver grain as described in any one of claim 1-3, it is characterised in that adjust
Conditioning agent used is NaOH either one of potassium hydroxide or ammoniacal liquor during section pH value.
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| CN201610821438.5A CN106623964B (en) | 2016-09-13 | 2016-09-13 | A kind of preparation method of tree Nano silver grain |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107127355A (en) * | 2017-07-04 | 2017-09-05 | 广东工业大学 | A kind of flower-shaped silver nanoparticle ball, its preparation method and its application |
| CN110935888A (en) * | 2019-11-01 | 2020-03-31 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of dendritic silver powder |
| CN114000348A (en) * | 2021-11-29 | 2022-02-01 | 华南理工大学 | Silver-plated conductive fabric and preparation method and application thereof |
| CN114951636A (en) * | 2022-07-11 | 2022-08-30 | 中国石油大学(华东) | Silver nano cube @ branch-shaped nano gold core-shell structure and preparation method and application thereof |
-
2016
- 2016-09-13 CN CN201610821438.5A patent/CN106623964B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107127355A (en) * | 2017-07-04 | 2017-09-05 | 广东工业大学 | A kind of flower-shaped silver nanoparticle ball, its preparation method and its application |
| CN107127355B (en) * | 2017-07-04 | 2019-07-19 | 广东工业大学 | A kind of flower-shaped silver nanoparticle ball, preparation method and its application |
| CN110935888A (en) * | 2019-11-01 | 2020-03-31 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of dendritic silver powder |
| CN110935888B (en) * | 2019-11-01 | 2022-07-01 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Preparation method of dendritic silver powder |
| CN114000348A (en) * | 2021-11-29 | 2022-02-01 | 华南理工大学 | Silver-plated conductive fabric and preparation method and application thereof |
| CN114000348B (en) * | 2021-11-29 | 2022-08-12 | 华南理工大学 | Silver-plated conductive fabric and preparation method and application thereof |
| CN114951636A (en) * | 2022-07-11 | 2022-08-30 | 中国石油大学(华东) | Silver nano cube @ branch-shaped nano gold core-shell structure and preparation method and application thereof |
| CN114951636B (en) * | 2022-07-11 | 2023-09-29 | 中国石油大学(华东) | Silver nanocube @ branch-shaped nano gold core-shell structure and preparation method and application thereof |
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| CN106623964B (en) | 2018-09-07 |
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