CN105618783A - Preparation method for silver nanoparticles with optical activity - Google Patents

Preparation method for silver nanoparticles with optical activity Download PDF

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Publication number
CN105618783A
CN105618783A CN201610009837.1A CN201610009837A CN105618783A CN 105618783 A CN105618783 A CN 105618783A CN 201610009837 A CN201610009837 A CN 201610009837A CN 105618783 A CN105618783 A CN 105618783A
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solution
preparation
nano silver
optical activity
silver grain
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王静
周伟
罗秦
费扬扬
文梦婷
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Jiangsu University of Science and Technology
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Jiangsu University of Science and Technology
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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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a preparation method for silver nanoparticles with the optical activity. The preparation method comprises the steps that a, a small biological molecule water solution with a certain concentration is prepared, after NaOH is added and the pH of the water solution is adjusted, a certain amount of silver nitrate is added (the silver nitrate and organic chiral small molecules are added into the solution according to a certain molar ratio), and a mixed solution is formed; b, the mixed solution is subjected to overnight aging after being added with a certain amount of polyvinylpyrrolidone (PVP); and c, then, a reducing agent NaBH4 solution is newly prepared in an ice-water bath, and the reducing agent solution is dropwise added under rapid magnetic stirring; finally, the color of the mixed solution becomes stable orange yellow, and it shows that the silver nanoparticles are generated in a reaction system. According to the preparation method for the silver nanoparticles with the optical activity, the method has important significance to the chiral research of nano materials, in particular to the research of chiral silver nano materials and also has important significance for manufacturing novel chiral nano sensors, parting materials and photoelectric functional devices.

Description

A kind of preparation method with optical activity Nano silver grain
Technical field
The invention belongs to liquid phase chemical field, be specifically related to a kind of preparation method with optical activity Nano silver grain.
Background technology
Metal nanoparticle becomes the perpetual object of many basic research and applied research with the optics of its uniqueness, electricity, magnetics, catalysis and chemical reaction character. In recent years, the special optical property of argent nanoparticle causes the great interest of people, and research shows that the chiral molecule being adsorbed on surfaces of metal nanoparticles can induce particle to produce optical activity. Chiral nanomaterial has a wide range of applications in fields such as chiral Recognition, chiral separation material, chiral sensor, chirality photoelectric functional device, chiral catalysis material, novel stealth materials. The conventional method preparing nanoparticle has chemical reduction method, phase transfer method, electrochemical process, sonochemical method and photochemical method. Compared with other method, liquid phase method has the advantages such as highly versatile, equipment is simple, technology is less demanding, is one of current laboratory and the industrial widely used method preparing nanoparticle. Circular dichroism spectra is a kind of special absorption spectra, and the conformation of its chiral molecule is very sensitive. Chirality is the key character of material, they be can not be overlapping Three-dimensional glass as enantiomer, although molecular formula is identical, but differently configured in space of its Atom or atomic radical, mirror image each other. Chiral molecule all has optical activity, and namely sample measured by available circular dichroism spectra instrument, thus obtaining the Chiral properties of sample.
Along with the fast development of nano material, the chirality research of nano material has become the focus that people pay close attention to. Although the preparation method basic research of Nano silver grain is ripe at present, but the preparation method and its chirality interaction mechanism, chiral Recognition, chiral nature and forming process etc. to exploration and optimization chirality Nano silver grain still awaits further research.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the present invention provides a kind of preparation method with optical activity Nano silver grain.
Technical scheme: for solving above-mentioned technical problem, a kind of preparation method with optical activity Nano silver grain provided by the invention, its preparation process includes:
A) prepare certain density biological micromolecule aqueous solution, after adding the NaOH pH value regulating solution, add a certain amount of silver nitrate (silver nitrate becomes certain mol proportion in the solution with the little molecule of organic chiral), form mixed solution; B) add mixed solution overnight ageing in above-mentioned mixed solution after a certain amount of polyvinylpyrrolidone (PVP); C) in ice-water bath, reducing agent NaBH is then newly prepared4Solution, under quick magnetic agitation, dropwise drips reductant solution, the color of final solution become stablize orange-yellow, it was shown that reaction system has Nano silver grain generate.
Further, described organic chiral small molecule solution is inosine, cytidine, adenosine or N-BETA-Alanyl-L-histidine solution.
Further, the concentration of described organic chiral small molecule solution is 0.1 ~ 5mmol L-1.
Further, the concentration of described silver nitrate solution is 0.2 ~ 5mmol L-1.
Further, in described mixed solution, biological micromolecule and Ag+ mol ratio are 10:1 ~ 1:4.
Further, described NaOH regulates pH value pH=7 ~ 10 of solution.
Further, described PVP molecular weight Mw=49000, PVP addition is 0 ~ 125mg.
Further, described NaBH4Solution is newly configured in ice-water bath.
Beneficial effect: the present invention in terms of existing technologies:
The present invention provides one to utilize the method that solution phase chemical reduction prepares the Nano silver grain with optical activity (chirality), the silver nano material with optical activity (chirality) has potential using value in fields such as chiral catalysis, asymmetric separation, chirality switch and chiral Recognition, therefore researchs and develops this kind of material and has very important significance. The preparation process that the present invention relates to is simple, and technology is less demanding, and cost is low. Adopting deionized water as solvent, with silver nitrate for raw material, the little molecule of organic chiral is as stabilizer and chiral induction agent, and sodium borohydride is as reducing agent, and by simple mixing, liquid-phase reduction has been prepared has optically active Nano silver grain.
Accompanying drawing explanation
The uv-visible absorption spectra figure of Nano silver grain prepared by Fig. 1.
The circular dichroism spectrogram of Nano silver grain prepared by Fig. 2 inosine system.
Fig. 3 is the circular dichroism spectrogram of the Nano silver grain that in embodiment 4 prepared by cytidine system.
Fig. 4 is the circular dichroism spectrogram of the Nano silver grain that in embodiment 5 prepared by adenosine system.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is further described.
Embodiment 1:
The preparation method with optical activity Nano silver grain, concrete preparation process is: taking concentration is 0.8mmol L-1Inosine aqueous solution 10mL, add NaOH regulate solution pH value be 7. Separately take 100 �� L20mmol L-1Silver nitrate aqueous solution join inosine aqueous solution, in mixed solution, the concentration of silver nitrate is 0.2mmol L-1, by mixed solution overnight ageing. To new compound concentration be 5mmol L in ice-water bath-1NaBH4, under quick magnetic agitation, dropwise it is added drop-wise in the mixed solution after ageing. When the color of solution becomes stable orange-yellow, it was shown that solution generates Nano silver grain. As it is shown in figure 1, be the uv-visible absorption spectra figure of Nano silver grain prepared by the present embodiment, there is an absworption peak at about 430nm in the Nano silver grain of preparation, is attributed to Nano silver grain surface plasmon absorption. Fig. 2 is the circular dichroism spectrogram of Nano silver grain prepared by the present embodiment. There is positive Cotton effect (CottonEffect) peak at 413nm in Nano silver grain, negative Cotton effect (CottonEffect) peak occurs at 491nm, shows as negative coupling. Show that Nano silver grain prepared by this system has chirality.
Embodiment 2:
The preparation method with optical activity Nano silver grain, concrete preparation process is: taking concentration is 0.1mmol L-1Inosine aqueous solution 10mL, the pH value adding NaOH adjustment solution is 7. Separately take 100 �� L20mmol L-1Silver nitrate aqueous solution join inosine aqueous solution, in mixed solution, the concentration of silver nitrate is 0.2mmol L-1, by mixed solution overnight ageing. To new compound concentration be 5mmol L in ice-water bath-1NaBH4, under quick magnetic agitation, dropwise it is added drop-wise in the mixed solution after ageing. When the color of solution becomes stable orange-yellow, it was shown that solution generates Nano silver grain.
Embodiment 3:
The preparation method with optical activity Nano silver grain, concrete preparation process is: taking concentration is 0.1mmol L-1Inosine aqueous solution 10mL, the pH value adding NaOH adjustment solution is 9.4. Separately take 100 �� L20mmol L-1Silver nitrate aqueous solution join inosine aqueous solution, in mixed solution, the concentration of silver nitrate is 0.2mmol L-1, by mixed solution overnight ageing. To new compound concentration be 5mmol L in ice-water bath-1NaBH4, under quick magnetic agitation, dropwise it is added drop-wise in the mixed solution after ageing. When the color of solution becomes stable orange-yellow, it was shown that solution generates Nano silver grain.
Embodiment 4:
The preparation method with optical activity Nano silver grain, concrete preparation process is: taking concentration is 0.2mmol L-1Cytidine aqueous solution 10mL, is added thereto to 100 �� L20mmol L-1Silver nitrate aqueous solution, in mixed solution, the concentration of silver nitrate is 0.2mmol L-1. 100mg polyvinylpyrrolidone (PVP, M is added in above-mentioned mixed solutionw=49000) by mixed solution overnight ageing. It is 5mmol L by the concentration of preparation new in ice-water bath-1NaBH4, under quick magnetic agitation, dropwise it is added drop-wise in the mixed solution after ageing. When the color of solution becomes stable orange-yellow, it was shown that solution generates Nano silver grain. As shown in Figure 3, it it is the circular dichroism spectrogram of Nano silver grain prepared by the present embodiment, there is negative Cotton effect (CottonEffect) peak at 380nm in Nano silver grain, positive Cotton effect (CottonEffect) peak occurs at 442nm, shows as positive coupling. Show that Nano silver grain prepared by this system has chirality.
Embodiment 5:
The preparation method with optical activity Nano silver grain, concrete preparation process is: taking concentration is 0.4mmol L-1Adenosine aqueous solution 10mL, is added thereto to 100 �� L20mmol L-1Silver nitrate aqueous solution, in mixed solution, the concentration of silver nitrate is 0.2mmol L-1. It is 5mmol L by the concentration of preparation new in ice-water bath-1NaBH4, under quick magnetic agitation, dropwise it is added drop-wise in the mixed solution after ageing. When the color of solution becomes stable orange-yellow, it was shown that solution generates Nano silver grain. As shown in Figure 4, being the circular dichroism spectrogram of Nano silver grain prepared by the present embodiment, there is positive Cotton effect (CottonEffect) peak at 426nm in Nano silver grain, corresponding to the plasmon absorption of nano grain of silver sub-surface. Show that under this condition, the Nano silver grain of preparation has good optical activity (chirality).
Embodiment 6:
The preparation method with optical activity Nano silver grain, concrete preparation process is: taking concentration is 0.2mmol L-1Carnosine aqueous solution 10mL, is added thereto to 100 �� L20mmol L-1Silver nitrate aqueous solution, in mixed solution, the concentration of silver nitrate is 0.2mmol L-1. 100mg polyvinylpyrrolidone (PVP, M is added in above-mentioned mixed solutionw=49000) by mixed solution overnight ageing. It is 5mmol L by the concentration of preparation new in ice-water bath-1NaBH4, under quick magnetic agitation, dropwise it is added drop-wise in the mixed solution after ageing. When the color of solution becomes stable orange-yellow, it was shown that solution generates Nano silver grain.
The above is only the preferred embodiment of the present invention; it is noted that, for those skilled in the art; under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (9)

1. a preparation method with optical activity Nano silver grain, it is characterised in that: its preparation process includes:
A) prepare certain density organic chiral micromolecular water solution, after adding the NaOH pH value regulating solution, add a certain amount of silver nitrate solution, form mixed solution; B) add mixed solution overnight ageing in above-mentioned mixed solution after a certain amount of polyvinylpyrrolidone; C) in ice-water bath, reducing agent NaBH is then newly prepared4Solution, under quick magnetic agitation, dropwise drips reductant solution, the color of final solution become stablize orange-yellow, it was shown that reaction system has Nano silver grain generate.
2. the preparation method with optical activity Nano silver grain according to claim 1, it is characterised in that: described organic chiral small molecule solution is inosine, cytidine, adenosine or N-BETA-Alanyl-L-histidine solution.
3. the preparation method with optical activity Nano silver grain according to claim 2, it is characterised in that: the concentration of described organic chiral small molecule solution is 0.1 ~ 5mmol L-1.
4. the preparation method with optical activity Nano silver grain according to claim 1, it is characterised in that: the concentration of described silver nitrate solution is 0.2 ~ 5mmol L-1.
5. the preparation method with optical activity Nano silver grain according to claim 2, it is characterised in that: in described mixed solution, biological micromolecule and Ag+ mol ratio are 10:1 ~ 1:4.
6. the preparation method with optical activity Nano silver grain according to claim 2, it is characterised in that: described NaOH regulates pH value pH=7 ~ 10 of solution.
7. the preparation method with optical activity Nano silver grain according to claim 2, it is characterised in that: described PVP molecular weight Mw=49000.
8. the preparation method with optical activity Nano silver grain according to claim 2, it is characterised in that: described PVP addition is 0 ~ 125mg.
9. the preparation method with optical activity Nano silver grain according to claim 2, it is characterised in that: described NaBH4The concentration of solution is 3.0 ~ 30mmol L-1, for newly configured in ice-water bath.
CN201610009837.1A 2015-01-28 2016-01-07 Preparation method for silver nanoparticles with optical activity Pending CN105618783A (en)

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CN105987894A (en) * 2016-07-06 2016-10-05 天津大学 Application of enzyme coupling nucleic acid-silver nanometer probe to D-amino acid detection
CN106018371A (en) * 2016-07-06 2016-10-12 天津大学 Enzyme-coupled nucleic acid-silver nanoprobe
CN106903326A (en) * 2017-01-23 2017-06-30 华南理工大学 Preparation method, UV type Nano silver conductive inks of spherical Nano Silver and preparation method thereof
CN110573280A (en) * 2017-04-28 2019-12-13 乐金显示有限公司 Metal nanostructure and method of making same
CN111266598A (en) * 2018-12-05 2020-06-12 同济大学 Preparation method of chiral metal nano spiral fiber array
CN111432965A (en) * 2017-12-15 2020-07-17 同和电子科技有限公司 Spherical silver powder and method for producing same

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105987894A (en) * 2016-07-06 2016-10-05 天津大学 Application of enzyme coupling nucleic acid-silver nanometer probe to D-amino acid detection
CN106018371A (en) * 2016-07-06 2016-10-12 天津大学 Enzyme-coupled nucleic acid-silver nanoprobe
CN106018371B (en) * 2016-07-06 2019-02-15 天津大学 Enzyme coupling nucleic acid-argentum nanometer probe
CN105987894B (en) * 2016-07-06 2019-03-05 天津大学 Application of enzyme coupling nucleic acid-silver nanoparticle probe in detection D- amino acid
CN106903326A (en) * 2017-01-23 2017-06-30 华南理工大学 Preparation method, UV type Nano silver conductive inks of spherical Nano Silver and preparation method thereof
CN110573280A (en) * 2017-04-28 2019-12-13 乐金显示有限公司 Metal nanostructure and method of making same
EP3702073A4 (en) * 2017-12-15 2021-08-04 Dowa Electronics Materials Co., Ltd. Spherical silver powder and method for producing same
CN111432965A (en) * 2017-12-15 2020-07-17 同和电子科技有限公司 Spherical silver powder and method for producing same
KR20200093657A (en) * 2017-12-15 2020-08-05 도와 일렉트로닉스 가부시키가이샤 Spherical silver powder and its manufacturing method
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CN111266598A (en) * 2018-12-05 2020-06-12 同济大学 Preparation method of chiral metal nano spiral fiber array
CN111266598B (en) * 2018-12-05 2022-06-21 同济大学 Preparation method of chiral metal nano spiral fiber array

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