CN107812957A - A kind of method that fluorescence silver nano-grain is prepared based on silver mirror reaction - Google Patents

A kind of method that fluorescence silver nano-grain is prepared based on silver mirror reaction Download PDF

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CN107812957A
CN107812957A CN201711012907.XA CN201711012907A CN107812957A CN 107812957 A CN107812957 A CN 107812957A CN 201711012907 A CN201711012907 A CN 201711012907A CN 107812957 A CN107812957 A CN 107812957A
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silver
grain
solution
silver nano
nano
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CN107812957B (en
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马春蕾
王�琦
唐建可
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Shanxi Qise Environmental Protection Technology Co.,Ltd.
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Taiyuan Institute of 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
    • 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
    • B22F2009/245—Reduction reaction in an Ionic Liquid [IL]

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • General Physics & Mathematics (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a kind of method that fluorescence silver nano-grain is prepared based on silver mirror reaction.This method comprises the following steps：Compound concentration is 5 ~ 25 mmol L‑1Silver ammino solution；Take bovine serum albumen solution to add silver ammino solution in beaker, be placed in water-bath, stand reaction；Reacted test solution is transferred in the bag filter of molecular cut off 2000, dialyse 36 ~ 48h；Test solution after dialysis is centrifuged, 10 ~ 20 min are centrifuged under 10000 ~ 12000 rpm rotating speeds, obtain silver nano-grain dispersion liquid.The inventive method is from bovine serum albumin as template and reducing agent, silver nano-grain is prepared based on silver mirror reaction principle in-situ reducing silver ammonia, reaction condition is gentle, equipment is simple, simple operation, without additional reducing agent, with green it is quick the advantages of, the silver nano-grain being prepared shows photoluminescent property.

Description

A kind of method that fluorescence silver nano-grain is prepared based on silver mirror reaction
Technical field
The present invention relates to a kind of method that fluorescence silver nano-grain is prepared based on silver mirror reaction, belongs to nano material and prepares skill Art field.
Background technology
Silver nano-grain due to the properties such as its excellent electronics, optics, catalysis, antibacterial be extensively studied for chemistry, The fields such as material, environment, medical science, life science.Fluorescent characteristic silver nano-grain has good anti-light bleaching and bio-compatible Property, therefore metal ion, biomolecule detection and imaging research can be widely used for.Therefore, fluorescent characteristic silver nano-grain Prepare it is significant.
Compared to traditional physics, chemical synthesis process, biological template method avoid using complex and expensive instrument and equipment and The high-temperature and high-pressure conditions of highly energy-consuming, there is the advantages of green low consumption, simple to operate.Bovine serum albumin is as a kind of cheap albumen Matter is widely used in the preparation of noble metal, metal oxide nano-material, therefore, silver nano material is prepared based on cow's serum Method is widely studied, in these preparation methods, it will usually additional reducing agent is introduced to aid in synthesizing, it is green in spite of some Green syt is realized in the use of chromatic rendition agent, but it is still one urgently to be resolved hurrily to find simple green method to prepare silver nano-grain Problem.At present, though having the method report that silver ammino solution prepares silver nano-grain as silver element source, there is not yet without additional The report of reducing agent one-step synthesis fluorescence silver nano-grain.
The content of the invention
The present invention is intended to provide fluorescence is made in a kind of method that fluorescence silver nano-grain is prepared based on silver mirror reaction, one-step method Silver nano-grain, this method are simple and environmentally-friendly.
The principle of the present invention：By the use of bovine serum albumin as biological template, while its reproducibility is utilized, without additional In the case of reducing agent, based on silver mirror reaction principle, in-situ reducing silver ammino solution, so as to which one-step method prepares silver nano-grain.
The invention provides a kind of method that fluorescence silver nano-grain is prepared based on silver mirror reaction, comprise the following steps：
1）Silver nitrate is taken in clean beaker, adding distilled water is completely dissolved it, and it is pale brown to producing that concentrated ammonia liquor is added dropwise dropwise Color precipitates, and continues dropwise addition concentrated ammonia liquor to precipitation and is completely dissolved, constant volume, prepares 5 ~ 25 mmol L-1Silver ammino solution；
2）Bovine serum albumen solution is taken to add step 1 in beaker）In silver ammino solution, be placed in 30 ~ 60oIn C water-bath, Stand 90 ~ 120 min of reaction；
The quality proportioning of silver and bovine serum albumin is 5.39 ~ 53.95 in silver ammino solution:1000；
3）By step 2）Middle test solution is transferred in the bag filter of molecular cut off 2000, and dialyse 36 ~ 48 h；
4）By step 3）Test solution after middle dialysis is centrifuged, and 10 ~ 20 are centrifuged under 10000 ~ 15000 rpm rotating speeds Min, obtain silver nano-grain dispersion liquid.
Above-mentioned steps 4）In, after being centrifuged, it is 3.6 ~ 11.7 nm that supernatant, which obtains particle size range, and average grain diameter is 5 Nm silver nano-grain dispersion liquid, redisperse after the precipitation for centrifuging to obtain separates, it is 18.2 ~ 58.8 nm to obtain particle size range, is put down Silver nano-grain dispersion liquid of the equal particle diameter in 24 nm.
The present invention is used as template and reducing agent by bovine serum albumin, utilizes silver mirror reaction principle, in-situ reducing silver ammonia system It is standby to obtain the silver nano-grain with fluorescent characteristic.By after dialysing and centrifuging, obtain particle size range in 3.6 ~ 11.7 nm and 18.2 ~ 58.8 nm two kinds of silver nano-grains.
Beneficial effects of the present invention：
This method is using bovine serum albumin as template and reducing agent, and based on silver mirror reaction principle, in-situ reducing silver ammonia obtains silver Nano particle, this method avoid the use of HTHP and additional reducing agent, equipment is simple, simple operation, synthesis green, obtain To silver nano-grain show good fluorescent characteristic, there is the potential that metal ion and small molecule analysis detect.
Brief description of the drawings
Fig. 1 is in embodiment 1, and bovine serum albumen solution and silver ammino solution are blended in 30,40,50,60oIt is quiet under C water-baths Put the product that 90 min of reaction are obtained and excite lower fluorogram in 390 nm；
Fig. 2 is in embodiment 2, and bovine serum albumen solution and various concentrations silver ammino solution are blended in 50oUnder C water-baths, reaction is stood The product that 90 min are obtained excites lower fluorogram in 390 nm；
Fig. 3 is in embodiment 3, and bovine serum albumen solution and silver ammino solution are blended in 50oUnder C water-baths, 120 min of reaction are stood Obtained product excites lower fluorogram in 390 nm；
Fig. 4 is in embodiment 4, and bovine serum albumen solution and silver ammino solution are blended in 50oUnder C water-baths, stand 90 min of reaction and obtain The silver nano-grain centrifuged supernatant arrived（a）With precipitation redisperse（b）Nano particle size phenogram；
Fig. 5 is in embodiment 4, and bovine serum albumen solution and silver ammino solution are blended in 50oUnder C water-baths, stand 90 min of reaction and obtain The transmission electron microscope TEM figures of the silver nano-grain arrived；A and b represents the situation of different amplification respectively；
Fig. 6 is in embodiment 4, and bovine serum albumen solution and silver ammino solution are blended in 50oUnder C water-baths, stand 90 min of reaction and obtain The high-resolution-ration transmission electric-lens HRTEM figures of the silver nano-grain arrived（a）Scheme with SEAD SAED（b）.
Fig. 7 is in embodiment 4, and bovine serum albumen solution and silver ammino solution are blended in 50oUnder C water-baths, reaction 90 is stood The full spectrograms of x-ray photoelectron power spectrum XPS for the silver nano-grain that min is obtained（a）With silver-colored open score figure（b）.
Embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment 1：
（1）Silver nitrate 0.06375g is taken in clean beaker, adding a small amount of distilled water is completely dissolved it, and dense ammonia is added dropwise dropwise Water continues dropwise addition concentrated ammonia liquor to precipitation and is completely dissolved, be settled to 25mL, prepare 15 mmol L to brown color precipitation is produced-1Silver Ammonia solution.
（2）2.5 g bovine serum albumins are weighed in beaker, constant volume obtains dense in 50 mL volumetric flasks after being dissolved in water Spend for 50 mg mL-1Bovine serum albumen solution, respectively take the mL of solution 5 in four beakers, then be separately added into 5mL steps 1） In silver ammino solution, be respectively placed in 30,40,50,60oIn C water-bath, 90 min of reaction are stood.Reaction obtains yellow solution, Wherein 30,40oProduct has an obvious muddiness under C, and 60oProduct has slight haze under C.
（3）Above-mentioned test solution is transferred in the bag filter of molecular cut off 2000, dialyse 36 h.Solution is dividing after taking dialysis Its fluorescence spectrum in the case where 390 nm are excited is determined on sub- fluorophotometric instrument.
Fig. 1 is using molecular fluorescence photometer（F-7000, FDAC）To above-mentioned 30,40,50,60oC is reacted Sample surveys its fluorescence spectrum in the case where 390 nm are excited, and obtains it and fluorescence peak, and 50 occurs in 490 nmoC reaction products are strong Degree is maximum.
（4）By step（3）Test solution after middle dialysis is centrifuged, and 10 min are centrifuged under 15000 rpm rotating speeds, Obtain silver nano-grain dispersion liquid.
Embodiment 2：
（1）Taking the g of silver nitrate 0.02125,0.06375,0.10625 respectively, adding a small amount of distilled water makes it in clean beaker It is completely dissolved, concentrated ammonia liquor is added dropwise dropwise to brown color precipitation is produced, continues dropwise addition concentrated ammonia liquor to precipitation and is completely dissolved, be settled to 25mL, prepare 5,15,25 mmol L-1Silver ammino solution.
（2）2.5 g bovine serum albumins are weighed in beaker, constant volume obtains dense in 50 mL volumetric flasks after being dissolved in water Spend for 50 mg mL-1Bovine serum albumen solution, take the solution 5 mL to add 5mL steps in beaker（1）Middle various concentrations Silver ammino solution, be placed in 50oIn C water-bath, 90 min of reaction are stood.
（3）Above-mentioned test solution is transferred in the bag filter of molecular cut off 2000, dialyse 48 h.Solution is dividing after taking dialysis Its fluorescence spectrum in the case where 390 nm are excited is determined on sub- fluorophotometric instrument.
Fig. 2 is using molecular fluorescence photometer（F-7000, FDAC）To above-mentioned 5,15,25 mmol L-1Silver-colored ammonia The fluorescence spectrum for the silver nano-grain that solution is prepared, maximum emission wavelength are respectively 456,475,490 nm.
（4）By step（3）Test solution after middle dialysis is centrifuged, and 20 min are centrifuged under 10000 rpm rotating speeds, Obtain silver nano-grain dispersion liquid.
Embodiment 3：
（1）The g of silver nitrate 0.06375 is taken in clean beaker, adding a small amount of distilled water is completely dissolved it, is added dropwise dropwise dense Ammoniacal liquor continues dropwise addition concentrated ammonia liquor to precipitation and is completely dissolved, be settled to 25 mL, prepare 15 mmol L to brown color precipitation is produced-1 Silver ammino solution.
（2）5.0 g bovine serum albumins are weighed in beaker, constant volume obtains dense in 50 mL volumetric flasks after being dissolved in water Spend for 100 mg mL-1Bovine serum albumen solution, take the solution 5 mL to add 5mL steps in beaker（1）Middle difference is dense The silver ammino solution of degree, is placed in 50oIn C water-bath, 120 min of reaction are stood.
（3）Above-mentioned test solution is transferred in the bag filter of molecular cut off 2000, dialyse 48 h.Solution is dividing after taking dialysis Its fluorescence spectrum in the case where 390 nm are excited is determined on sub- fluorophotometric instrument.
Fig. 3 is using molecular fluorescence photometer（F-7000, FDAC）The above-mentioned min of reaction 120 is prepared The fluorescence spectra of silver nano-grain, maximum emission wavelength are 475 nm.
（4）By step（3）Test solution after middle dialysis is centrifuged, and 20 min are centrifuged under 12000 rpm rotating speeds, Obtain silver nano-grain dispersion liquid.
Embodiment 4：
（1）Silver nitrate 0.06375g is taken in clean beaker, adding a small amount of distilled water is completely dissolved it, and dense ammonia is added dropwise dropwise Water continues dropwise addition concentrated ammonia liquor to precipitation and is completely dissolved, be settled to 25mL, prepare 15 mmol L to brown color precipitation is produced-1Silver Ammonia solution.
（2）2.5 g bovine serum albumins are weighed in beaker, constant volume obtains dense in 50 mL volumetric flasks after being dissolved in water Spend for 50 mg mL-1Bovine serum albumen solution, take the solution 5 mL to add 5mL steps in beaker（1）In silver-colored ammonia it is molten Liquid, it is placed in 50oIn C water-bath, 90 min of reaction are stood.
（3）Above-mentioned test solution is transferred in the bag filter of molecular cut off 2000, dialyse 48 h.
（4）By step（3）Test solution after middle dialysis centrifuges 15 min under 15000 rpm rotating speeds, and supernatant obtains light Yellow solution, redisperse after the precipitation for centrifuging to obtain separates, determines its nano particle size respectively.
Fig. 4 is using Malvern nano particle size instrument（Nano-ZS90, Malvern）Centrifuged supernatant and precipitation are divided again Dissipate the test result of solution.As a result show,（a）The particle size range of silver nano-grain is 3.6 ~ 11.7 nm in supernatant, average grain Footpath is 5 nm,（b）The particle size range of the silver nano-grain of precipitation after distribution is 18.2 ~ 58.8 nm, and average grain diameter is in 24 nm.
Fig. 5 is using transmission electron microscope（Tecnai-G20, U.S. FEI）Above-mentioned silver nano-grain is characterized Result.It is apparent that silver nano-grain is spherical, and the distribution of two kinds of sizes be present.
Fig. 6 is using transmission electron microscope（Tecnai-G20, U.S. FEI）High score is carried out to above-mentioned silver nano-grain Distinguish the result characterized with SEAD.This it appears that the lattice and diffraction spot of silver nano-grain, it was demonstrated that silver nanoparticle Particle has good crystallinity.
Fig. 7 is using x-ray photoelectron spectroscopy（K-Alpha, U.S.'s match is silent to fly）Table is carried out to above-mentioned silver nano-grain The result of sign, show that the material is made up of elements such as C 1s, O 1s, N 1s, Ag 3d, wherein in 374.3 Hes in Ag 3d open scores Swarming at 368.3 eV corresponds respectively to Ag 3d3/2With Ag 3d5/2。

Claims (4)

  1. A kind of 1. method that fluorescence silver nano-grain is prepared based on silver mirror reaction, it is characterised in that：Comprise the following steps：
    1）Silver nitrate is taken in clean beaker, adding distilled water is completely dissolved it, and it is pale brown to producing that concentrated ammonia liquor is added dropwise dropwise Color precipitates, and continues dropwise addition concentrated ammonia liquor to precipitation and is completely dissolved, constant volume, prepares 5 ~ 25 mmol L-1Silver ammino solution；
    2）Bovine serum albumen solution is taken to add step 1 in beaker）Obtained silver ammino solution, is placed in 30 ~ 60oC water-bath In, stand 90 ~ 120 min of reaction；
    3）By step 2）Middle test solution is transferred in the bag filter of molecular cut off 2000, and dialyse 36 ~ 48 h；
    4）By step 3）Test solution after middle dialysis is centrifuged, and 10 ~ 20 are centrifuged under 10000 ~ 15000 rpm rotating speeds Min, obtain silver nano-grain.
  2. 2. the method according to claim 1 that fluorescence silver nano-grain is prepared based on silver mirror reaction, it is characterised in that：Step 2）In, using bovine serum albumin as template and reducing agent, bovine serum albumin used is biological level, in mixed silver ammino solution silver with The quality proportioning of bovine serum albumin is 5.39 ~ 53.95:1000.
  3. 3. the method according to claim 1 that fluorescence silver nano-grain is prepared based on silver mirror reaction, it is characterised in that：Ox blood The concentration of albumin soln is 50 ~ 100 mg mL-1。
  4. 4. the method according to claim 1 that silver nano-grain is prepared based on silver mirror reaction, it is characterised in that：Step 4） In, after being centrifuged, supernatant is collected, obtains silver nano-grain dispersion liquid of the particle diameter in 3.6 ~ 11.7 nm, it is heavy after centrifugation Redisperse after the separation of shallow lake, obtains silver nano-grain dispersion liquid of the particle diameter in 18.2 ~ 58.8 nm.
CN201711012907.XA 2017-10-26 2017-10-26 Method for preparing fluorescent silver nanoparticles based on silver mirror reaction Active CN107812957B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109319842A (en) * 2018-09-29 2019-02-12 山西大学 A kind of fast preparation method of the manganese dioxide nano particle of bovine serum albumin load
CN114848819A (en) * 2022-06-09 2022-08-05 大连大学 Preparation method and application of photosensitive silver nano chitosan microspheres

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CN102515276A (en) * 2011-12-30 2012-06-27 四川大学 Method for preparing manganese dioxide nanoparticles with bovine serum albumin as template
CN104985193A (en) * 2015-07-24 2015-10-21 天津大学 Alloy nano-particle preparation method based on protein reduction method
EP3028792A1 (en) * 2014-12-02 2016-06-08 Institute Of Chemistry, Chinese Academy Of Sciences Nano-silver powder, the preparation method and application in preparation of electrically conductive ink of the same and electrically conductive ink
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Publication number Priority date Publication date Assignee Title
CN102515276A (en) * 2011-12-30 2012-06-27 四川大学 Method for preparing manganese dioxide nanoparticles with bovine serum albumin as template
EP3028792A1 (en) * 2014-12-02 2016-06-08 Institute Of Chemistry, Chinese Academy Of Sciences Nano-silver powder, the preparation method and application in preparation of electrically conductive ink of the same and electrically conductive ink
CN104985193A (en) * 2015-07-24 2015-10-21 天津大学 Alloy nano-particle preparation method based on protein reduction method
CN107116232A (en) * 2017-06-14 2017-09-01 江南大学 A kind of synthetic method of pltine nano-cluster

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109319842A (en) * 2018-09-29 2019-02-12 山西大学 A kind of fast preparation method of the manganese dioxide nano particle of bovine serum albumin load
CN114848819A (en) * 2022-06-09 2022-08-05 大连大学 Preparation method and application of photosensitive silver nano chitosan microspheres
CN114848819B (en) * 2022-06-09 2024-02-09 大连大学 Preparation method and application of photosensitive silver nano chitosan microsphere

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