CN108971512A - A kind of the green preparation and its application of the rectangular particle of porous spongy Ag - Google Patents

A kind of the green preparation and its application of the rectangular particle of porous spongy Ag Download PDF

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Publication number
CN108971512A
CN108971512A CN201811071545.6A CN201811071545A CN108971512A CN 108971512 A CN108971512 A CN 108971512A CN 201811071545 A CN201811071545 A CN 201811071545A CN 108971512 A CN108971512 A CN 108971512A
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rectangular
particle
spongy
solution
porous
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CN108971512B (en
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门丹丹
张洪华
向军淮
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Jiangxi Science and Technology Normal University
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Jiangxi Science and Technology Normal University
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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
    • 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
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • 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
    • 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
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • 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]

Abstract

It is applied the present invention relates to the green preparation of field of nanometer material technology more particularly to a kind of rectangular particle of porous spongy Ag and its in near-infrared SERS, proposes sodium borohydride (NaBH4) reduction silver orthophosphate (Ag3PO4) the rectangular method received particle, prepare the rectangular particle of porous spongy Ag, the spongy rectangular particle of micro-structure Ag prepared by the present invention, near-infrared exist it is strong absorb, near-infrared SERS detection may be implemented.It solves during Raman test, if using visible light that can bury in oblivion the Raman signal of target molecule due to strong light scattering and fluorescence background as excitation wavelength, and then the problem of leading to biggish detection error and low detection sensitivity, achieve substantive progress.

Description

A kind of the green preparation and its application of the rectangular particle of porous spongy Ag
Technical field
The present invention relates to the green preparation of field of nanometer material technology more particularly to a kind of rectangular particle of porous spongy Ag and its Using.
Background technique
Porous noble metal (such as Au, Ag) nano particle is since there are tables for big specific surface area, high load capacity and near-infrared The performances such as face plasma resonance (Surface Plasmon Resonance, SPR) electro-catalysis, medicament slow release, bio-imaging, The numerous areas such as Surface enhanced Raman scattering (SERS) have a good application prospect.
Currently, porous or biscuit micro/nano material the method for synthesis is mainly template and dealloying corrosion method. Such as, it is multiple to have synthesized spongiform silver, gold, copper, silver-copper oxide and silver-titanium dioxide using glucan as soft template by Walsh et al. Condensation material.This method is although fairly simple, inexpensive and environmentally friendly, but needs higher calcination temperature (600 DEG C -900 DEG C). In addition, the typically small (< 2m of specific surface area of the mat gold metal nano-particle prepared by template2/ g), answer its practical With being restricted.Dealloying corrosion method is first synthesis precious metal alloys nano particle (such as: Au-Ag), later by de- alloy Process (chemistry or electrochemical method) prepares porous metals nano particle.In this method, the preparation of precious metal alloys nano particle Generally pass through wet chemistry method.And in wet chemistry method preparation process, surfactant is inevitably used, not only will affect mesh The absorption of molecule is marked, while being also possible to generate interference to the Raman signal of target molecule.In the recent period, Li seminar proposes with single layer two Dimension colloidal crystal is template, deposited metal layer, high annealing, de- alloy process synthetic sponge shape metal nanoparticle.This method Solve the problems, such as wet chemistry method preparation nano particle there are surfactants.Based on this method, which is successfully prepared Spongy Au-Ag, Au-Cu, Au-Ag-Cu alloy nanoparticle array.However, this method yield is lower (can only once to prepare one layer Spongy nano particle), and need (600-1000 DEG C) of high temperature annealing.Recently, Yin and Wang seminar is about spongy The synthesis of metal nano material achieves biggish achievement, and solving wet chemistry method, there are surfactants and Colloidal Template Method to produce Low problem is measured, but used methods are relative complex (needing multilayer coating structure and multistep reaction), reaction condition is also more severe It carves (high annealing).
To solve the above problems, present applicant proposes sodium borohydride (NaBH4) reduction silver orthophosphate (Ag3PO4) rectangular receive Grain, the method for preparing the rectangular particle of porous spongy Ag.This method is simple, quick, environmentally friendly, economical, and whole process is without using table Face activating agent and high-temperature process.
Summary of the invention
For conventional method prepare spongy porous noble metal nano particles complex process, there are surfactant, compare table The deficiencies of area is small, the present invention provides a kind of green, simple, economic methods to prepare the rectangular particle of porous spongy Ag, and It is had studied in the application of near-infrared SERS.
The environment-friendly preparation method thereof of the heretofore described rectangular particle of porous spongy Ag, comprising the following specific steps
(1) [Ag (NH is prepared3)2]+Solution: 0.45M ammonia spirit is instilled into 2mL 0.45M dropwise under stirring conditions AgNO3In solution, until solution becomes clarification, [Ag (NH is obtained3)2]+Solution.
(2) [Ag (NH for preparing (1)3)2]+Solution instills in 100mL deionized water, later by 1mL 0.15M's Na2HPO4Aqueous solution instills above-mentioned [Ag (NH3)2]+In solution, 10min is persistently stirred, obtains rectangular Ag through centrifugation3PO4Nanometer Grain, appearance are dark brown to smear.
(3) by Ag3PO4Rectangular nano particle is scattered in again in 10mL water, instills the NaBH of the 0.5M of 50 μ L4Aqueous solution, Be stirred to react about 2-5min it is uniform after, obtain the rectangular particle of porous spongy Ag.
The rectangular particle of Ag prepared by the present invention is applied to: using this spongy rectangular particle of micro-structure Ag as substrate, for giving birth to The detection of the SERS of compound matter.
The rectangular particle of porous spongy Ag prepared by the present invention, because its large specific surface area, porosity Gao Erneng are dramatically increased Local enhances object to be measured molecular amounts within the scope of electric field action, while highdensity " heat can also be generated between nano-pore Point " exists in infrared band and absorbs, is a kind of good near-infrared SERS substrate.
Beneficial effects of the present invention
(1) method that the embodiment of the present invention proposes the spongy rectangular particle of micro-structure Ag of preparation, the conjunction with the prior art It is compared at method, there is reaction condition mildly (room temperature), environmental protection (reaction carries out in aqueous solution) is easy to operate, efficient, and Grain clean surface, pole are conducive to absorption and the follow-up function of target molecule.
(2) there is strong absorption in near-infrared, may be implemented close in the spongy rectangular particle of micro-structure Ag prepared by the present invention Infrared SERS detection.It solves during Raman test, if using visible light as excitation wavelength, since strong light dissipates It penetrates and fluorescence background, the Raman signal of target molecule can be buried in oblivion, and then cause biggish detection error and low detection sensitive The problem of spending achieves substantive progress.
(3) present invention is by being added suitable NaBH4Additional amount so that preparation have the rectangular particle-surface of spongy Ag Heart cubic structure.
Detailed description of the invention
Fig. 1 is the preparation process figure of the rectangular particle of porous spongy micro-structure Ag；
Fig. 2 is the electron scanning micrograph of the rectangular particle of porous spongy Ag obtained；
Fig. 3 is the rectangular particle X-ray energy spectrum diagram of spongy Ag；
Fig. 4 is X-ray diffraction (XRD) map of the rectangular particle of spongy Ag；
Fig. 5 is different NaBH4Additional amount preparation the rectangular particle of porous spongy Ag, scanning electron microscope observation after The SEM photograph of shooting；
Fig. 6 is the rectangular particle absorption spectrum characterization of spongy Ag；
Fig. 7 is the various concentration 4-ATP (10 measured using the rectangular nano particle of spongy Ag as substrate-6M-10-11M) SERS spectrogram.
In order to more clearly from show technical solution provided by the present invention and generated technical effect, below with tool Body embodiment is provided for the embodiments of the invention the rectangular granular materials of porous spongy Ag and near-infrared SERS detection is retouched in detail It states.
Embodiment 1
Process flow chart as shown in the accompanying drawings 1, a kind of rectangular particle of porous spongy micro-structure Ag, use are following Step is prepared:
Step a, [Ag (NH is prepared first3)2]+Solution: 0.45M ammonium hydroxide is instilled 0.45M's dropwise under stirring conditions AgNO3In solution, until solution becomes clarification, [Ag (NH is obtained3)2]+Solution；Later by the [Ag (NH of preparation3)2]+Solution instills In 100mL deionized water, stir evenly.By the Na of 1mL 0.15M2HPO4Aqueous solution instills above-mentioned [Ag (NH3)2]+In solution, hold Continuous stirring 10-20min, obtains rectangular Ag through centrifugation3PO4Nano particle, appearance are dark brown to smear.
Step b, by Ag3PO4Rectangular nano particle is scattered in again to be instilled in 10mL deionized water, and the 0.5M of 50 μ L is instilled NaBH4Aqueous solution, normal-temperature reaction 2-5min are centrifuged, and the rectangular particle of porous spongy Ag is obtained.
Further, to rectangular of the porous spongy micro-structure Ag prepared according to the step of embodiments of the present invention 1 Grain, is scanned electron micrograph, absorption spectrum and raman spectroscopy measurement, specific testing result is as follows respectively:
(1) using 200 field emission scanning electron microscope of Sirion to porous made from step b in the embodiment of the present invention 1 The spongy rectangular particle of Ag is observed, and shoots (the SEM figure of the electron scanning micrograph as shown in Figure of description 2 Picture)；Wherein, Fig. 2 a is the rectangular particle of low power porous spongy Ag, by it can be seen that being prepared for dispersing uniform rectangular particle. Particle is in porous spongy structure, and similar multiple nanometer rods intersect (see Fig. 2 b and Fig. 2 c).Further by its high power figure (figure It 2d) can be seen that the nanometer rods for constituting Ag micro-structural framework are made of multiple little particles.Due to NaBH4Restore Ag3PO4In the process, First generate small nano particle, later the fused formation nanometer rods of small nano particle and caused by.
(2) X- that the spongy rectangular particle of micro-structure Ag obtained is obtained with Inca.Oxford type X-ray energy disperse spectroscopy Radial energy spectrogram (EDS), is shown in Figure of description 3.By EDS it is found that the component of the rectangular particle of porous spongy Ag is Ag member Plain (Si element is from Si substrate).
(3) by after on the rectangular even particulate dispersion to glass slide of porous spongy Ag obtained, with German Bruker D8- Advance type x-ray diffractometer carries out X-ray diffraction (XRD) map of test acquisition to it, sees figure Figure of description 4.Its In, map ordinate is opposite diffracted intensity, and abscissa is the angle of diffraction.XRD data are shown, through NaBH4After reduction, Ag3PO4's Structural characteristic peak disappears, and apparent Ag face-centred cubic structure characteristic peak occurs, it was demonstrated that the particle of acquisition is Ag particle, with EDS As a result consistent.
(4) Fig. 5 is different NaBH4Additional amount preparation porous spongy Ag rectangular particle 200 Flied emission of Sirion The SEM photograph shot after scanning electron microscope observation.As seen from the figure, when be added NaBH4 additional amount be respectively 5 μ L (Fig. 5 a) and When 15 μ L (Fig. 5 b), the Ag nano particle of generation dispersedly divides in Ag3PO4Particle surface there is no the porous spongy side Ag Shape nano particle.Further increase NaBH4Additional amount when being 25 μ L (Fig. 5 c), the Ag nano particle of generation increases, but Ag3PO4 It still has.When the additional amount for continuing to increase NaBH4 is 100 μ L (Fig. 5 d), rectangular of porous spongy Ag can get Grain, in NaBH4Additional amount is that the 50 μ L rectangular particle of porous spongy Ag (see Fig. 2) obtained is compared, and pattern is without significant change. These results suggest that NaBH4Additional amount it is most important to preparing for the rectangular particle of spongy Ag.NaBH4Additional amount it is less when, Only in Ag3PO4Produce Ag nano particle；And with NaBH4Additional amount increase, the Ag nano particle of generation gradually increases. This is because NaBH4Addition, Ag3PO4It is reduced, generates Ag core.Generating Ag core becomes nuclearing centre, and then is grown to serve as Ag Nano particle.So the yield and NaBH of Ag core4Additional amount it is proportional, with NaBH4Additional amount increase, generate Ag nano particle gradually increase.In addition, working as concentration NaBH4When lower, the Ag nano particle of formation can not merge in time, thus The rectangular particle of spongy Ag can not be constructed；Work as NaBH4Additional amount when reaching a certain concentration, the Ag nano particle of formation can and Shi Ronghe, to be built into the rectangular particle of porous spongy Ag.
(5) absorption spectrum characterization is carried out to the spongy rectangular particle of micro-structure Ag with Cary 500, sees Figure of description 6, Wherein, map abscissa is wavelength (unit nm), and ordinate is intensity.It absorbs map and shows that this spongy rectangular Ag receives Rice grain, absorption spectrum, there are other than the intrinsic SPR absorption peak of Ag, are deposited in addition at 400nm in visible light and near infrared region In a wide absorption band.This is because the spongy rectangular grain structure of Ag is made of Ag nanometer rods intersection, so entire sponge Shape particle network structure has length dimension, it is made to all show SPR phenomenon in entire visible light region and near infrared region.
(6) Figure of description 7 is to use micro- Confocal laser-scanning microscopy instrument (Nexus, Nicolet), with 4- aminobenzene sulphur Phenol (4-ATP) is probe molecule, and excitation wavelength 785nm is measured different dense using the rectangular nano particle of spongy Ag as substrate Spend 4-ATP (10-6M-10-11M SERS spectrogram).Wherein map abscissa is wave number (unit cm-1), ordinate is intensity. As seen from the figure, the spongy rectangular nano particle substrate of Ag is to concentration down to 10-10The 4-ATP of M SERS still with higher is sensitive Property, show that the structure has very high SERS activity.

Claims (2)

1. a kind of green preparation of rectangular particle of porous spongy Ag, which is characterized in that be prepared using following steps:
(1) [Ag (NH is prepared3)2]+Solution: 0.45M ammonium hydroxide is instilled to the AgNO of 0.45M dropwise under stirring conditions3In solution, Until solution becomes clarification, [Ag (NH is obtained3)2]+Solution；
(2) by [Ag (NH of preparation3)2]+Solution instills in 100mL deionized water, stirs evenly, by the Na of 2mL 0.15M2HPO4 Aqueous solution instills above-mentioned [Ag (NH3)2]+In solution, 20min is persistently stirred, obtains rectangular Ag through centrifugation3PO4Nano particle, outside It sees dark brown to smear；
(3) by Ag3PO4Rectangular nano particle is scattered in again in 10mL aqueous solution, instills the NaBH of the 0.5M of 50 μ L4Aqueous solution, Normal-temperature reaction 2-5min is centrifuged, and the rectangular particle of spongy Ag is obtained.
2. a kind of application of the rectangular particle of porous spongy Ag, it is characterised in that: using this spongy rectangular particle of Ag as substrate, use In the detection of the SERS of biochemical substances.
CN201811071545.6A 2018-09-14 2018-09-14 Green preparation method and application of porous spongy Ag square particles Expired - Fee Related CN108971512B (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101731268A (en) * 2008-11-17 2010-06-16 尖端奈米科技股份有限公司 Nano silver porous material and manufacturing method thereof
US20110014300A1 (en) * 2008-05-05 2011-01-20 Jawaharlal Nehru Centre For Advanced Scientfic Res Template Free and Polymer Free Metal, Nanosponge and a Process Thereof
CN102296349A (en) * 2011-07-06 2011-12-28 上海大学 De-alloying preparation method of nanometer porous metal substrate with surface enhanced Raman scattering activity
CN102910608A (en) * 2012-10-25 2013-02-06 常州大学 Preparation method of porous silver phosphate catalyst
CN104368340A (en) * 2014-12-01 2015-02-25 应城市武瀚有机材料有限公司 Sponge silver catalyst preparation method and application of sponge silver catalyst to oxidation and synthesis of cinnamic acid from cinnamaldehyde
CN105624456A (en) * 2016-03-22 2016-06-01 北京航空航天大学 Spongy superfine nanometer porous metal and preparation method
CN106670495A (en) * 2015-11-06 2017-05-17 南京大学 Preparation method of network-state Ag-Au-Pd trimetal porous material
CN107043096A (en) * 2017-05-23 2017-08-15 河南科技学院 A kind of nanometer spherical Ag3PO4And its preparation method and application

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110014300A1 (en) * 2008-05-05 2011-01-20 Jawaharlal Nehru Centre For Advanced Scientfic Res Template Free and Polymer Free Metal, Nanosponge and a Process Thereof
CN101731268A (en) * 2008-11-17 2010-06-16 尖端奈米科技股份有限公司 Nano silver porous material and manufacturing method thereof
CN102296349A (en) * 2011-07-06 2011-12-28 上海大学 De-alloying preparation method of nanometer porous metal substrate with surface enhanced Raman scattering activity
CN102910608A (en) * 2012-10-25 2013-02-06 常州大学 Preparation method of porous silver phosphate catalyst
CN104368340A (en) * 2014-12-01 2015-02-25 应城市武瀚有机材料有限公司 Sponge silver catalyst preparation method and application of sponge silver catalyst to oxidation and synthesis of cinnamic acid from cinnamaldehyde
CN106670495A (en) * 2015-11-06 2017-05-17 南京大学 Preparation method of network-state Ag-Au-Pd trimetal porous material
CN105624456A (en) * 2016-03-22 2016-06-01 北京航空航天大学 Spongy superfine nanometer porous metal and preparation method
CN107043096A (en) * 2017-05-23 2017-08-15 河南科技学院 A kind of nanometer spherical Ag3PO4And its preparation method and application

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