CN105798322A - Preparation method and application of silver nanocluster - Google Patents
Preparation method and application of silver nanocluster Download PDFInfo
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- CN105798322A CN105798322A CN201610152251.0A CN201610152251A CN105798322A CN 105798322 A CN105798322 A CN 105798322A CN 201610152251 A CN201610152251 A CN 201610152251A CN 105798322 A CN105798322 A CN 105798322A
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- silver nanoclusters
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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
- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
Abstract
The invention provides a preparation method of a silver nanocluster. The prepared silver nanocluster has high purity and high fluorescence intensity, and is uniform and good in reproducibility. The preparation method is simple, feasible and fast. Raw materials are wide in source and low in price, the preparation process is free of pollution, and the preparation method can be used for large-scale industrialized production. The prepared silver nanocluster is sensitive to the pH value, the fluorescence intensity is enhanced along with the increase of pH, and it is shown that the silver nanocluster can be used as a fluorescence switch to indicate pH changes in a system.
Description
Technical field
The present invention relates to silver nanoclusters synthetic technology, particularly relate to preparation method and the application thereof of a kind of silver nanoclusters.
Background technology
In the last few years, with various template molecule and stabilizer such as protein, DNA, the reagent such as mercaptan was the focus that the water miscible fluorescence metal nano-cluster of Material synthesis becomes research.In the process of synthesis, it is necessary to use substantial amounts of template molecule and stabilizer, and these molecules likely can with a lot of analyte qualitative responses, thus follow-up detection is caused very big puzzlement.And the inner filtering effect of synthetic raw material also can reduce the fluorescence of synthesized bunch.So water-soluble nano bunch be purified to the emphasis in order to work at present.As far as we know, 3 kinds of methods are currently mainly adopted to carry out purifying nano bunch: dialysis, ultrafiltration and chromatographic separation technology.And these methods purify more complicated comparatively speaking, time-consuming, refining effect is unsatisfactory.
The change of pH value is the important mark weighing living organism physiological change, closely bound up with the field of scientific study such as modern medicine, biological engineering.The method of the change measuring pH value is a lot, such as acidometer, fluorescent material etc..Fluorimetry adopts the change instruction pH value of fluorescence parameter, easy, quick, sensitivity is good, and exploitation is used for detecting living things system H+The pH fluorescent probe of change has broad application prospects in biomedical research.In this patent, we are prepared for the fluorescence nano bunch that pH is sensitive, and adopt a kind of simple method-sedimentation method to purify silver nanoclusters.
Summary of the invention
It is an object of the invention to provide the preparation method of the silver nanoclusters of a kind of high-purity, high fluorescent and application thereof.
In order to achieve the above object, on the one hand, the preparation method that the invention provides a kind of silver nanoclusters, it is characterised in that: it comprises the following steps:
Step 1, prepares the aqueous solution of bovine serum albumin or thioctic acid；
Step 2, adds in the aqueous solution of step 1 by solvable silver salt, mix homogeneously, then adds solvable BH4 -Saline solution, stirring prepares silver nanoclusters stock solution；
Step 3, adds acid solution in the silver nanoclusters stock solution that step 2 obtains, is 3-6 to pH value, obtains silver nanoclusters precipitation；
Step 4, silver nanoclusters step 3 obtained precipitates by centrifugation, separates, washes, is more again dispersed in the alkaline solution that pH value is 9-12.
On the other hand, the silver nanoclusters adopting method described in first aspect present invention to prepare, it is applied to detection living things system H+The pH fluorescent probe of change.
The invention has the beneficial effects as follows: the preparation method of silver nanoclusters provided by the present invention, the silver nanoclusters prepared has high-purity, high fluorescent；The silver nanoclusters prepared is more uniform, favorable reproducibility；Preparation method is simple, and quickly, material source is extensively cheap, and preparation process is pollution-free, can be used for large-scale industrial production；Silver nanoclusters prepared by the present invention, the increase fluorescence intensity to pH sensitive, along with pH strengthens, it was shown that silver nanoclusters can as the change of pH in fluorescent switch directive system.
Detailed description of the invention
On the one hand, the preparation method that the invention provides a kind of silver nanoclusters, it is characterised in that: it comprises the following steps:
Step 1, prepares the aqueous solution of bovine serum albumin or thioctic acid；
Step 2, adds in the aqueous solution of step 1 by solvable silver salt, mix homogeneously, then adds solvable BH4 -Saline solution, stirring prepares silver nanoclusters stock solution；
Step 3, adds acid solution in the silver nanoclusters stock solution that step 2 obtains, is 3-6 to pH value, obtains silver nanoclusters precipitation；
Step 4, silver nanoclusters step 3 obtained precipitates by centrifugation, separates, washes, is more again dispersed in the alkaline solution that pH value is 9-12.
Preferably, in described step 1, prepare the aqueous solution of thioctic acid, also include step 5, the dispersion liquid of step 4 will add solvable BH4 -Saline solution, stirring prepares silver nanoclusters.
Preferably, described step 1 is prepared the aqueous solution of thioctic acid, the Ag of every 1 molfraction in step 2+The corresponding BH adding 4-6 molfraction4 -；Or, step 1 is prepared the aqueous solution of bovine serum albumin, the Ag of every 1 molfraction+The corresponding BH adding 0.1-0.4 molfraction4 -。
Preferably, described step 1 is prepared the aqueous solution of thioctic acid, the Ag of every 1 molfraction in step 2+The corresponding thioctic acid adding 12-16 molfraction；Or, step 1 is prepared the aqueous solution of bovine serum albumin, the Ag of every 1 mass fraction+The corresponding bovine serum albumin adding 26-34 mass fraction.
Preferably, in described step 3, acid solution is HNO3Or HAc, concentration is 0.1-1M.
Preferably, in described step 4, centrifugal speed is that 10000-12000 turns/min.
Preferably, the deionized water of washing 5-10mL in described step 4, cleans 3-5 time.
Preferably, described step 2 and solvable BH in step 54 -Salt is NaBH4, concentration is 1mM-1M.
Preferably, in described step 5, mixing time is 3-24h.
On the other hand, the silver nanoclusters adopting method described in first aspect present invention to prepare, it is applied to detection living things system H+The pH fluorescent probe of change.
Below in conjunction with specific embodiment, the preparation method of silver nanoclusters of the present invention is described further.
Embodiment 1
(1) bovine serum albumin is dissolved the solution forming clear in aqueous；
(2) by AgNO3Add in solution, mix homogeneously, form mixed material, wherein, the Ag of every 1 mass fraction+The corresponding bovine serum albumin adding 30 mass fractions；
(3) under stirring, it is slowly added dropwise sodium hydroxide solution and sodium borohydride, continues 6 hours prepared silver nanoclusters stock solution of stirring, wherein, the Ag of every 1 molfraction+The corresponding BH adding 0.2 molfraction4 -；
(4) in stock solution, add 0.1MHAc, regulate the pH to 3-6 of silver nanoclusters stock solution, promote the generation of silver nanoclusters precipitation；
(5) silver nanoclusters is deposited under the 10000-12000 rotating speed turned centrifugal, separates, then the deionized water of precipitation 5-10mL is cleaned 3 times；
(6) precipitation after cleaned being dispersed in alkaline solution solution again that form clear, the pH value of alkaline solution prepares silver nanoclusters between 9-12.
To the silver nanoclusters prepared at ambient temperature, adopting spectrofluorophotometer test equipment test product fluorescence quantum yield is 2.2%.
To the silver nanoclusters prepared at ambient temperature, adopt spectrofluorophotometer test product to purify the fluorescence ratio of front and back, be 95%.
Embodiment 2
(1) bovine serum albumin is dissolved the solution forming clear in aqueous；
(2) by AgNO3Add in solution, mix homogeneously, form mixed material, wherein, the Ag of every 1 mass fraction+The corresponding bovine serum albumin adding 26 mass fractions；
(3) under stirring, it is slowly added dropwise sodium hydroxide solution and sodium borohydride, continues 6 hours prepared silver nanoclusters stock solution of stirring, wherein, the Ag of every 1 molfraction+The corresponding BH adding 0.1 molfraction4 -；
(4) in stock solution, add 0.5MHAc, regulate the pH to 3-6 of silver nanoclusters stock solution, promote the generation of silver nanoclusters precipitation；
(5) silver nanoclusters is deposited under the 10000-12000 rotating speed turned centrifugal, separates, then the deionized water of precipitation 5-10mL is cleaned 3 times；
(6) precipitation after cleaned being dispersed in alkaline solution solution again that form clear, the pH value of alkaline solution prepares silver nanoclusters between 9-12.
To the silver nanoclusters prepared at ambient temperature, adopting spectrofluorophotometer test equipment test product fluorescence quantum yield is 2.0%.
To the silver nanoclusters prepared at ambient temperature, adopt spectrofluorophotometer test product to purify the fluorescence ratio of front and back, be 90%.
Embodiment 3
(1) bovine serum albumin is dissolved the solution forming clear in aqueous；
(2) by AgNO3Add in solution, mix homogeneously, form mixed material, wherein, the Ag of every 1 mass fraction+The corresponding bovine serum albumin adding 34 mass fractions；
(3) under stirring, it is slowly added dropwise sodium hydroxide solution and sodium borohydride, continues 6 hours prepared silver nanoclusters stock solution of stirring, wherein, the Ag of every 1 molfraction+The corresponding BH adding 0.4 molfraction4 -；
(4) in stock solution, add 1MHAc, regulate the pH to 3-6 of silver nanoclusters stock solution, promote the generation of silver nanoclusters precipitation；
(5) silver nanoclusters is deposited under the 10000-12000 rotating speed turned centrifugal, separates, then the deionized water of precipitation 5-10mL is cleaned 3 times；
(6) precipitation after cleaned being dispersed in alkaline solution solution again that form clear, the pH value of alkaline solution prepares silver nanoclusters between 9-12.
To the silver nanoclusters prepared at ambient temperature, adopting spectrofluorophotometer test equipment test product fluorescence quantum yield is 2.1%.
To the silver nanoclusters prepared at ambient temperature, adopt spectrofluorophotometer test product to purify the fluorescence ratio of front and back, be 93%.
Embodiment 4
(1) it is dissolved in alkaline aqueous solution by thioctic acid to be formed the solution of clear；
(2) by AgNO3Add in solution, mix homogeneously, form mixed material, wherein, the Ag of every 1 molfraction+The corresponding thioctic acid adding 14 molfractions；
(3) under stirring, it is slowly added dropwise sodium borohydride solution in mixed material, continues 6 hours prepared silver nanoclusters stock solution of stirring, wherein, the Ag of every 1 molfraction+The corresponding BH adding 5 molfractions4 -；
(4) in stock solution, 0.1MHNO is added3, regulate the pH to 3-6 of silver nanoclusters stock solution, promote the generation of silver nanoclusters precipitation；
(5) silver nanoclusters is deposited under the 10000-12000 rotating speed turned centrifugal, separates, then the deionized water of precipitation 5-10mL is cleaned 4 times；
(6) precipitation after cleaned being dispersed in alkaline solution solution again that form clear, the pH value of alkaline solution is between 9-12.
To the silver nanoclusters prepared at ambient temperature, adopting spectrofluorophotometer test equipment test product fluorescence quantum yield is 2.5%.
To the silver nanoclusters prepared at ambient temperature, adopt spectrofluorophotometer test product to purify the fluorescence ratio of front and back, be 108%.
Embodiment 5
(1) it is dissolved in alkaline aqueous solution by thioctic acid to be formed the solution of clear；
(2) by AgNO3Add in solution, mix homogeneously, form mixed material, wherein, the Ag of every 1 molfraction+The corresponding thioctic acid adding 12 molfractions；
(3) under stirring, it is slowly added dropwise sodium borohydride solution in mixed material, continues 6 hours prepared silver nanoclusters stock solution of stirring, wherein, the Ag of every 1 molfraction+The corresponding BH adding 4 molfractions4 -；
(4) in stock solution, 0.5MHNO is added3, regulate the pH to 3-6 of silver nanoclusters stock solution, promote the generation of silver nanoclusters precipitation；
(5) silver nanoclusters is deposited under the 10000-12000 rotating speed turned centrifugal, separates, then the deionized water of precipitation 5-10mL is cleaned 4 times；
(6) precipitation after cleaned being dispersed in alkaline solution solution again that form clear, the pH value of alkaline solution is between 9-12.
To the silver nanoclusters prepared at ambient temperature, adopting spectrofluorophotometer test equipment test product fluorescence quantum yield is 2.3%.
To the silver nanoclusters prepared at ambient temperature, adopt spectrofluorophotometer test product to purify the fluorescence ratio of front and back, be 105%.
Embodiment 6
(1) it is dissolved in alkaline aqueous solution by thioctic acid to be formed the solution of clear；
(2) by AgNO3Add in solution, mix homogeneously, form mixed material, wherein, the Ag of every 1 molfraction+The corresponding thioctic acid adding 16 molfractions；
(3) under stirring, it is slowly added dropwise sodium borohydride solution in mixed material, continues 6 hours prepared silver nanoclusters stock solution of stirring, wherein, the Ag of every 1 molfraction+The corresponding BH adding 6 molfractions4 -；
(4) in stock solution, 1MHNO is added3, regulate the pH to 3-6 of silver nanoclusters stock solution, promote the generation of silver nanoclusters precipitation；
(5) silver nanoclusters is deposited under the 10000-12000 rotating speed turned centrifugal, separates, then the deionized water of precipitation 5-10mL is cleaned 4 times；
(6) precipitation after cleaned being dispersed in alkaline solution solution again that form clear, the pH value of alkaline solution is between 9-12.
To the silver nanoclusters prepared at ambient temperature, adopting spectrofluorophotometer test equipment test product fluorescence quantum yield is 2.4%.
To the silver nanoclusters prepared at ambient temperature, adopt spectrofluorophotometer test product to purify the fluorescence ratio of front and back, be 106%.
Embodiment 7
(1) it is dissolved in alkaline aqueous solution by thioctic acid to be formed the solution of clear；
(2) by AgNO3Add in solution, mix homogeneously, form mixed material, wherein, the Ag of every 1 molfraction+The corresponding thioctic acid adding 16 molfractions；
(3) under stirring, it is slowly added dropwise sodium borohydride solution in mixed material, continues 6 hours prepared silver nanoclusters stock solution of stirring, wherein, the Ag of every 1 molfraction+The corresponding BH adding 6 molfractions4 -；
(4) in stock solution, 0.1MHNO is added3, regulate the pH to 3-6 of silver nanoclusters stock solution, promote the generation of silver nanoclusters precipitation；
(5) silver nanoclusters is deposited under the 10000-12000 rotating speed turned centrifugal, separates, then the deionized water of precipitation 5-10mL is cleaned 5 times；
(6) precipitation after cleaned being dispersed in alkaline solution solution again that form clear, the pH value of alkaline solution is between 9-12；
(7) in above-mentioned solution, 1mM-1MNaBH is added4, stirring 3-24h prepares silver nanoclusters.
To the silver nanoclusters prepared at ambient temperature, adopting spectrofluorophotometer test equipment test product fluorescence quantum yield is 2.1%.
To the silver nanoclusters prepared at ambient temperature, adopt spectrofluorophotometer test product to purify the fluorescence ratio of front and back, be 110%.
The foregoing is only the better embodiment of the present invention, not in order to limit invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a silver nanoclusters, it is characterised in that: it comprises the following steps:
Step 1, prepares the aqueous solution of bovine serum albumin or thioctic acid；
Step 2, adds in the aqueous solution of step 1 by solvable silver salt, mix homogeneously, then adds solvable BH4 -Saline solution, stirring prepares silver nanoclusters stock solution；
Step 3, adds acid solution in the silver nanoclusters stock solution that step 2 obtains, is 3-6 to pH value, obtains silver nanoclusters precipitation；
Step 4, silver nanoclusters step 3 obtained precipitates by centrifugation, separates, washes, is more again dispersed in the alkaline solution that pH value is 9-12.
2. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: in described step 1, prepare the aqueous solution of thioctic acid, also include step 5, the dispersion liquid of step 4 will add solvable BH4 -Saline solution, stirring prepares silver nanoclusters.
3. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: described step 1 is prepared the aqueous solution of thioctic acid, the Ag of every 1 molfraction in described step 2+The corresponding BH adding 4-6 molfraction4 -；Or, step 1 is prepared the aqueous solution of bovine serum albumin, the Ag of every 1 molfraction+The corresponding BH adding 0.1-0.4 molfraction4 -。
4. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: described step 1 is prepared the aqueous solution of thioctic acid, the Ag of every 1 molfraction in described step 2+The corresponding thioctic acid adding 12-16 molfraction；Or, step 1 is prepared the aqueous solution of bovine serum albumin, the Ag of every 1 mass fraction+The corresponding bovine serum albumin adding 26-34 mass fraction.
5. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: in described step 3, acid solution is HNO3Or HAc, concentration is 0.1-1M.
6. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: in described step 4, centrifugal speed is that 10000-12000 turns/min.
7. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: the deionized water of washing 5-10mL in described step 4, cleans 3-5 time.
8. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: described step 2 and solvable BH in step 54 -Salt is NaBH4, concentration is 1mM-1M.
9. the preparation method of silver nanoclusters as claimed in claim 1, it is characterised in that: in described step 5, mixing time is 3-24h.
10. the silver nanoclusters adopting method described in claim 1 to prepare, is applied to detection living things system H+The pH fluorescent probe of change.
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Cited By (6)
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| CN106891016A (en) * | 2017-01-10 | 2017-06-27 | 青岛科技大学 | A kind of preparation of fluorescence silver nanoclusters and its method for manifesting latent fingerprint |
| CN106984826A (en) * | 2016-11-17 | 2017-07-28 | 湖南科技大学 | A kind of method for the silver nanoclusters that preparation of pH regulation and control is launched with hyperfluorescence |
| CN107011527A (en) * | 2017-05-04 | 2017-08-04 | 长春工业大学 | A kind of preparation method and application of the silver nanoclusters of temperature-responsive/polyalcohol hydrogel composite |
| CN107018991A (en) * | 2017-04-26 | 2017-08-08 | 江南大学 | A kind of antibacterial film of silver-colored lysozyme nano-cluster modification |
| CN109001281A (en) * | 2018-09-03 | 2018-12-14 | 湖北大学 | A kind of molecular engram optical electro-chemistry sensor and its preparation method and application based on organic and inorganic quantum dot P-N heterojunction structure |
| CN111208099A (en) * | 2020-01-08 | 2020-05-29 | 同济大学 | Silver nano-cluster fluorescent probe, preparation method thereof and application thereof in detection of active oxygen species |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106984826A (en) * | 2016-11-17 | 2017-07-28 | 湖南科技大学 | A kind of method for the silver nanoclusters that preparation of pH regulation and control is launched with hyperfluorescence |
| CN106891016A (en) * | 2017-01-10 | 2017-06-27 | 青岛科技大学 | A kind of preparation of fluorescence silver nanoclusters and its method for manifesting latent fingerprint |
| CN107018991A (en) * | 2017-04-26 | 2017-08-08 | 江南大学 | A kind of antibacterial film of silver-colored lysozyme nano-cluster modification |
| CN107018991B (en) * | 2017-04-26 | 2020-05-08 | 江南大学 | Antibacterial film modified by silver-lysozyme nanoclusters |
| CN107011527A (en) * | 2017-05-04 | 2017-08-04 | 长春工业大学 | A kind of preparation method and application of the silver nanoclusters of temperature-responsive/polyalcohol hydrogel composite |
| CN109001281A (en) * | 2018-09-03 | 2018-12-14 | 湖北大学 | A kind of molecular engram optical electro-chemistry sensor and its preparation method and application based on organic and inorganic quantum dot P-N heterojunction structure |
| CN111208099A (en) * | 2020-01-08 | 2020-05-29 | 同济大学 | Silver nano-cluster fluorescent probe, preparation method thereof and application thereof in detection of active oxygen species |
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| CN105798322B (en) | 2018-04-24 |
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