CN106623964B - A kind of preparation method of tree Nano silver grain - Google Patents
A kind of preparation method of tree Nano silver grain Download PDFInfo
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- CN106623964B CN106623964B CN201610821438.5A CN201610821438A CN106623964B CN 106623964 B CN106623964 B CN 106623964B CN 201610821438 A CN201610821438 A CN 201610821438A CN 106623964 B CN106623964 B CN 106623964B
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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 a kind of green synthesis methods of novel tree-like structure Nano silver grain, under the conditions of one kind is intended to provide existing for no template, using cysteine or glutathione as reducing agent and agent of attaching the names of pre-determined candidates, tree Nano silver grain is quickly and easily prepared, this method reaction condition is mild, easy to operate, environmental pollution is small, and simple thinking is provided to prepare anisotropic nano-particle.Its basic scheme includes the following steps：1) reducing agent and argentiferous metal salt are weighed respectively；2) dissolving metal salts that step 1) weighs are prepared into aqueous metal salt in distilled water, reducing agent dissolves in distilled water；3) by aqueous metal salt in step 2) and reducing agent solution in molar ratio 1~5:5 mixing, adjust pH value 67 be stirred to react in thermostat water bath a period of time to get.
Description
Technical field
The present invention relates to the technical fields of nano material, and in particular to a kind of preparation of novel tree-like structure Nano silver grain
Method.
Background technology
Nano material refers at least one-dimensional in nanoscale range (being usually 1~100nm) in three dimensions
Grain or the material being made of as basic unit them.Nano particle can be divided into three classes substantially：(1) zero dimension refers to three dimensions
Scale is in nanoscale, such as spherical nanoparticle；(2) one-dimensional, referring to space has bidimensional to be in nanoscale, such as nano wire
(line), nanometer rods (bar), nanotube etc.；(3) two-dimentional, refer in three dimensions have it is one-dimensional in nanoscale, wherein including just nanometer
Piece, nano thin-film etc..In in the past few decades, people have synthesized the noble metal nano grain of different-shape using a variety of methods
Son systematically has studied the physics, chemistry and optical characteristics of noble metal nano particles, explores the microcosmic life of metal nanoparticle
Long mechanism develops them in catalysis, photonic propulsion, plasma optics, optical sensing, biomarker, medical imaging, Yi Jibiao
Face enhances all various function and applications such as Raman spectrum, achieves many important progress, also becomes this field and grinds
Study carefully hot spot.
Tree nano-particle is to pass through a kind of nano-particle assembling knot made of ordered fabrication by single nano-particle
Structure is single nano-particle by aligning, and forms dendritic structure.Its more traditional distributed nano-particle has richer
Rich optical characteristics and electronics property has a wide range of applications in the nano-devices such as manufacture electronics, photoelectron and sensor
Foreground.The synthesis of traditional tree metal nanoparticle is nearly all based on template assemblies, however, no matter molten
The ligand molecular soft template of the offer identification or interaction that are used in liquid, or the hard template based on the surface of solids,
All it is necessary to metal nanoparticle space structure assembling process, but template, there are chemical reagent pollution, reaction step is numerous
The defects of trivial, product are difficult to realize large-scale practical application, in biomedicine field using also restrained.
Against the above deficiency, under the conditions of the purpose of the present invention is to provide one kind existing for no template, half Guang is utilized
As reducing agent and activating agent, a step obtains tree Nano silver grain for propylhomoserin or reductive glutathione.This method is reacted
Mild condition, easy to operate, environmental pollution is small, has important application value in modern science field.
Invention content
The invention discloses a kind of green synthesis methods of novel tree-like structure Nano silver grain, it is desirable to provide one kind is not having
Under the conditions of having existing for template, using 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, this method reaction condition is mild, easy to operate, and environmental pollution is small, for system
Standby anisotropic nano-particle provides simple thinking.
The preparation method of tree Nano silver grain of the present invention, includes the following steps：
1) reducing agent and argentiferous metal salt are weighed respectively；
2) dissolving metal salts that step 1) weighs are prepared into metal salt solution, reducing agent dissolves in distilled water；
3) by reducing agent solution in step 2) and metal salt solution in molar ratio 1~5:5 mixing, adjust pH value 6-7,70
Be stirred to react in DEG C thermostat water bath 4h to get.
The environment-friendly preparation method thereof of above-mentioned tree Nano silver grain, the metal salt solution are that silver nitrate is dissolved in steaming
One of silver nitrate aqueous solution or silver ammino solution that distilled water obtains；The reducing agent is cysteine or reproducibility
One of glutathione；When adjusting pH value conditioning agent used be sodium hydroxide either potassium hydroxide or ammonium hydroxide wherein it
One.
During the present invention prepares tree Nano silver grain, by studying for a long period of time for inventor, set
The molar ratio of material molar ratio and reaction condition prepared by shape structure Nano silver grain, reducing agent and silver ion is to synthesizing tree-like knot
The Nano silver grain of structure is most important；The control of reaction condition such as temperature, pH and whether there is or not whipping process etc., to tree
The formation of nano-particle will produce apparent influence.The amount that L-cys is added in mixed system is different, the Nano silver grain of synthesis
Size and shape also difference.By changing the molar ratio of L-cys and silver nitrate, silver nanoparticle of different shapes can be obtained
Particle.The molar ratio of L-cys/Ag+ is less than 3:When 5, observation Electronic Speculum collection of illustrative plates does not show the presence of nano-particle；Work as L-cys/Ag
+ molar ratio be 4:When 5, spherical shape or spherical is presented in obtained silver nano-grain mostly, and not enough silver atoms are gone back
Original out forms dendritic structure；When gradually increasing to 5 with the molar ratio of L-cys/Ag+:5, nano-particle at this time is presented
Dendroid.
Compared with prior art, under the conditions of technical solution provided by the invention is existing for no template, half Guang ammonia is utilized
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, it is environmental-friendly, it is easy to operate, it is energy saving.It is reported that easy fresh breeze, Tae Gwan Park et al. are also prepared for setting
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 have more abundant light compared with metal nanoparticle and reguline metal
Characteristic and electronics property are learned, especially when manufacturing the nano-devices such as electronics, photoelectron and sensor, has and widely answers
With；Also the large-scale application of metal nanoparticle biologic medical detection field can be realized.
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 implementation mode
For a better understanding of the present invention with reference to specific embodiments the present invention is further explained.It should be understood that following
Embodiment only illustrates the present invention, rather than for limiting the scope of the invention.Unmentioned experimental method in embodiment, usually according to
Conventional method operates.
Embodiment 1
121mg cysteines accurately are weighed, are dissolved in 100ml distilled water solutions, the half Guang ammonia of 10mmol/L is configured to
Acid solution accurately weighs 170mg silver nitrates, distills water dissolution with 100ml, is configured to the silver nitrate solution of 10mmol/L.
To 5mL under the conditions of T=70 DEG C of temperature and pH=6.5,5ml is added in the silver nitrate solution of 10mmol/L,
The cysteine solution of 10mmol/L, is thoroughly stirred to react 4h, and the nanoparticles solution of brown color, and constant volume finally can be obtained
To 10mL.Device is whisked come controlling reaction temperature with constant temperature magnetic force in reaction process.
Embodiment 2
307.3mg reductive glutathiones accurately are weighed, is dissolved in 100ml distilled water solutions, is configured to 10mmol/L
Reductive glutathione solution, accurately weigh 170mg silver nitrates, with 100ml distill water dissolution, be configured to the nitre of 10mmol/L
Sour silver solution.
To 5mL under the conditions of T=70 DEG C of temperature and pH=6.5,2ml is added in the silver nitrate solution of 10mmol/L,
The reductive glutathione solution of 10mmol/L, is thoroughly stirred to react 4h, and the nanoparticles solution of brown color finally can be obtained,
And it is settled to 10mL.Device is whisked come controlling reaction temperature with constant temperature magnetic force in reaction process.
Embodiment 3
121mg cysteines accurately are weighed, are dissolved in 100ml distilled water solutions, the half Guang ammonia of 10mmol/L is configured to
Acid solution accurately weighs 170mg silver nitrates, with 10%100ml ammonia solvents, is configured to the silver ammino solution of 10mmol/L.
To 5mL under the conditions of T=70 DEG C of temperature and pH=6.5,5ml, 10mmol/ is added in the silver ammino solution of 10mmol/L
The cysteine solution of L, is thoroughly stirred to react 4h, and the nanoparticles solution of brown color finally can be obtained, and is settled to 10mL.
Device is whisked come controlling reaction temperature with constant temperature magnetic force in reaction process.
Embodiment 4
307.3mg reductive glutathiones accurately are weighed, is dissolved in 100ml distilled water solutions, is configured to 10mmol/L
Reductive glutathione solution, accurately weigh 170mg silver nitrates, with 10%100ml ammonia solvents, be configured to 10mmol/L's
Silver ammino solution.
To 5mL under the conditions of T=70 DEG C of temperature and pH=6.5,3ml, 10mmol/ is added in the silver ammino solution of 10mmol/L
The reductive glutathione solution of L, is thoroughly stirred to react 4h, and the nanoparticles solution of brown color, and constant volume finally can be obtained
To 10mL.Device is whisked come controlling reaction temperature with constant temperature magnetic force in reaction process.
The present invention uses cysteine green syt tree Nano silver grain, whole process not to use any adjuvant
And derivant, prepared tree Nano silver grain are coated by the oxidation product of cysteine, effectively increase nanometer
The stability and biocompatibility of particle.Now by taking tree Nano silver grain prepared in embodiment 1 as an example, in conjunction with 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 shows apparent 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, is cysteine or its oxidation product through infared spectrum validating analysis, is played stabilization.It is right above
Specific embodiments of the present invention are described.It is to be appreciated that the present invention is not limited to the above specific embodiments, this
Field technology personnel can make various deformations or amendments within the scope of the claims, this has no effect in the essence of the present invention
Hold.
Claims (3)
1. a kind of preparation method of tree Nano silver grain, which is characterized in that include the following steps：
1）Reducing agent and argentiferous metal salt are weighed respectively；The reducing agent is its of cysteine or reductive glutathione
One of；
2）By step 1）The dissolving metal salts weighed prepare metal salt solution, and reducing agent dissolves in distilled water；
3）By step 2）Middle reducing agent solution and metal salt solution in molar ratio 5:5 mixing, adjust pH
Value 6-7, be stirred to react in 70 DEG C of thermostat water baths 4h to get.
2. a kind of preparation method of tree Nano silver grain as described in claim 1, which is characterized in that the gold
It is that silver nitrate is dissolved in one of silver nitrate aqueous solution or the silver ammino solution that distilled water obtains to belong to salting liquid.
3. a kind of preparation method of tree Nano silver grain as claimed in claim 1 or 2, which is characterized in that adjust
Conditioning agent used is sodium hydroxide either one of potassium hydroxide or ammonium hydroxide when pH values.
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| 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 |
| 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 |
| CN114000348B (en) * | 2021-11-29 | 2022-08-12 | 华南理工大学 | Silver-plated conductive fabric 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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