CN102296349A - De-alloying preparation method of nanometer porous metal substrate with surface enhanced Raman scattering activity - Google Patents
De-alloying preparation method of nanometer porous metal substrate with surface enhanced Raman scattering activity Download PDFInfo
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Abstract
The invention relates to a de-alloying preparation method of a nanometer porous metal substrate with surface enhanced Raman scattering activity. The invention comprises the following steps: cutting an AB(C) alloy ribbon prepared by a single roller melt-spinning method into a length of 2-3 cm; putting the ribbon into a container filled with a electrolyte solution, heating the container from room temperature; respectively heating the container into different temperatures and performing heat preservation; observing the condition of bubbles of the reaction of active metal and the electrolyte solution, stopping the heat preservation when no obvious bubbles are observed, taking out the alloy ribbon from the electrolyte solution; flushing the alloy ribbon with anhydrous alcohol and deionized water; preparing a dilute organic matter solution as a probe molecule for Raman testing, soaking the substrate material in the probe molecule solution, taking the substrate material out, repeatedly flushing the substrate material with distilled water, and drying in air. The substrate obtained by the invention has a unique three-dimensional continuous nanometer porous structure, low technical cost, simple operation control, excellent surface enhancement effect, and has active engineering application value for the Raman enhancement field.
Description
Technical field
The present invention relates to a kind of nano porous metal substrate and simple, easy-operating removal alloying method preparation method thereof of surface-enhanced Raman scattering activity, belong to laser Raman spectroscopy detection technique field.
Background technology
As the common method of analyzing molecules vibrational spectrum, the laser raman technology has been widely used in mineral, jewel, medicine, foodstuff additive, chemical reagent detection, fields such as the molecular structure of discriminating material, the surperficial bonding state of analysis.Yet the Raman scattering effect signal often very a little less than, less when the concentration of tested molecule, or when surperficial adsorbent surveyed, conventional laser Raman method just seemed unable to do what one wishes, need be by auxiliary enhanced means.
(Surface-enhanced Raman Scattering spectroscopy SERS) is exactly a kind of Raman reinforcing effect to surface enhanced Raman scattering.When the molecular adsorption with resonance Raman(RR)effect when having the silver of uneven surface, gold or copper surperficial, the molecule Raman effect is enhanced, this phenomenon is called surface enhanced Raman scattering effect.Since last century, the seventies was found, surface enhanced Raman scattering effect has obtained broad research as a kind of high-sensitive surface analysis Detection Techniques in fields such as Surface Science, bio-science, at aspects such as katalysis, electrochemistry, bio-sensing and corrosion wide application prospect is arranged all.
Preparation has high surperficial reinforcing effect, and the enhancing substrate of good circulation ratio and stability is the prerequisite that application surface strengthens Raman scattering effect.The method that strengthens substrate for preparing commonly used, a kind of is to utilize chemistry or electrochemical method to make the metallic surface roughening, obtains having the uneven surface of high-ratio surface, the chemistry or the electrochemical process that prepare this substrate are difficult to control; Another kind method is the metal-sol that preparation has nanoscale, load there is metal-sol particulate substrate as strengthening substrate, the problem that this preparation method exists is that the nanoparticle aggregate phenomenon is uncontrollable, and the process that colloidal sol is dripped on the sheet glass does not have repeatability; Also having a kind of method in addition is the metallic membrane that has uneven surface by the method preparation of sputter or evaporation, and this method is to the requirement harshness of equipment.Therefore need carry out the research of the manageable preparation method simple to operation with the substrate of Raman reinforcing effect.
The removal alloying method is the method simple to operation of the metal of nano-porous structure with unique three-dimensional co-continuous of the preparation that causes extensive concern in recent years.The removal alloying method, also claim the selective corrosion method, be meant under the electropotential between the alloy constituent element differs bigger situation, the active element of the electrochemical properties in the alloy under electrolytical effect optionally dissolving enter electrolytic solution and stay the corrosion process of electrochemical properties than stable element.Constituent element both can be a kind of element in the single phase solid solution alloy, can be again a certain phase in the polyphase alloy.Remaining comparatively inert atoms metal is through the final nano-porous structure that forms co-continuous of the growth of reuniting.The new alloy system for preparing nano porous metal about removal alloying was developed gradually in recent years, such as Ni-Cu, Mn-Cu, Si-Pt, Al-Au, Pd-Ni-P etc., handle by removal alloying these systems, can be prepared into nano porous palladium (Nanoporous Pd, NPPd), nano-porous gold (Nanoporous Au, NPG), (Nanoporous Ag NPS) waits nano porous metal to nano-porous silver.Unique nano-porous structure is given big specific surface area of metal and nanometer size effect, and these characteristics combine with the Raman reinforcing effect of silver, gold, copper excellence itself, will give material more excellent nanometer reinforcing effect.
There are some researches show that the Raman that has nano-scale structure strengthens the scattering substrate, reinforcing effect can change along with the variation of microtexture size.Therefore the present invention is that virgin alloy, 5 wt.% HCl are electrolyte solution with the Al-Ag alloy, respectively 55 ± 2 in the preparation of nano porous metal
oC, 72 ± 2
oC, 98 ± 2
oThe nano-porous silver that preparation has different skeleton sizes under the C temperature is substrate with the nano-porous silver, with 10
-5(Crystal Violet, CV) solution has proposed concrete operational path for the Raman reinforcing effect of probe atom research NPS substrate to the Viola crystallina of M simultaneously.The present patent application people adopt nanoporous+removal alloying+Raman strengthen (nanoporous+dealloy+SERS) as keyword retrieval United States Patent (USP) digest (USPTO), European patent digest (EP-PCT), " Chinese patent Information Network " and " State Intellectual Property Office of the People's Republic of China's patent retrieval " are not found patent family.
Summary of the invention
The purpose of this invention is to provide a kind of removal alloying legal system Raman of getting everything ready that utilizes and strengthen the method for the active nano porous metal substrate of scattering.More particularly, the purpose of this invention is to provide and a kind ofly place electrolyte solution to carry out chemical corrosion AB (C) alloy to be that removal alloying is handled, to obtain having the preparation method that Raman strengthens the active nano porous metal substrate of scattering.
Removal alloying preparation method with the active nano porous metal substrate of Raman enhancing scattering of the present invention is achieved by following technique means:
Described AB (C) alloy, it is characterized in that between the alloying element or the alloy constituent element between have difference in Electrode Potential, and it is the precious metal element with Raman reinforcing effect that a kind of element is wherein arranged, such as Au-Ag, Ni-Cu, Mn-Cu, Al-Au, Al-Ag class alloy system.
Described electrolyte solution is characterized in that and more active element or constituent element in the alloy system can be dissolved, and do not influence the precious metal constituent element, such as can select hydrochloric acid, sulfuric acid based dilute acid soln or sodium hydroxide class dilute alkaline soln according to alloy system.
Preparation has removal alloying preparation technology and the activity test method thereof that Raman strengthens the active nano porous metal substrate of scattering, it is characterized in that having following processing step:
A. it is long to be cut into 2-3cm with AB (C) alloy thin band that single roller revolves the method preparation of quenching; AB (C) alloy is Al-Au, Al-Ag, Al-Cu, Mg-Ag, Mg-Ag-Pd;
B. strip is put into container, electrolyte solution is housed in the container, container begins to be heated by room temperature simultaneously; Described electrolyte solution is the aqueous hydrochloric acid of 5wt.%;
C. container is heated to differing temps and insulation respectively;
D. observe the bubble situation of active metal and electrolyte solution reaction in the container, wait not have obvious visible bubble in bubble, stop to be incubated, with alloy thin band by taking out in the electrolyte solution;
E. will wash 3-5 time with raw spirit through the alloy thin band of said process, use deionized water rinsing 3-5 time subsequently; Finally obtain the nanoporous precious metal in AB (C) alloy: nano-porous gold (NPG) or nano-porous silver (NPS) or nano porous palladium (NPPd);
F. dispose the probe molecule of certain density rare organic solution, take out base material is soaked 2h in probe molecule solution after, dry after washing repeatedly with distilled water as the Raman test.
The mechanism of the inventive method is: removal alloying prepares dissolving that nano porous metal relates to active element becomes the co-continuous of three-dimensional perforation with the diffusion aggregation of residue precious metal constituent element atoms metal nano-porous structure.There is special electromagnetic coupled between the skeleton of the nano-scale of contact each other in this nano-porous structure, have very strong adsorption in addition between micro-content organism molecule and the precious metal, the two makes the nanoporous precious metal can be used as at the bottom of the excellent Raman enhancing scattering active group.
The inventive method is applicable to multiple alloy system, and as the removal alloying process of alloy systems such as Au-Ag, Ni-Cu, Mn-Cu, Al-Au, Al-Ag, promptly multiple nano porous metal is as the preparation of NPG, NPPd, NPS etc.; At the bottom of can be used as the Raman enhancing scattering active group that detects a lot of micro-content organisms by the nano porous metal of this method preparation, as 10
-5The Viola crystallina of M (Crystal Violet, CV), 10
-6The rhodamine B of M (Rhodamine-B) etc.
Description of drawings
Fig. 1 be Al-25at.%Ag virgin alloy strip and in the 5wt.% of differing temps HCl solution the XRD curve behind the removal alloying.As seen Al-25 at.% Ag alloy thin band has all been realized removal alloying process completely in the electrolyte solution of differing temps.
Fig. 2 is Al-25 at.% Ag alloy thin band section SEM photo of gained NPS behind the removal alloying in the 5wt.% of differing temps HCl solution.Wherein Fig. 2 a) and b) be 55 ± 2
oThe section SEM photo of NPS behind the removal alloying in the 5wt.% HCl solution of C; Fig. 2 c) and d) be 72 ± 2
oThe SEM photo of NPS after the 5wt.% HCl solution interalloyization of C; Fig. 2 e) and f) be 98 ± 2
oThe SEM photo of NPS after the 5wt.% HCl solution interalloyization of C.Fig. 2 is a) for the SEM photo under amplifying 3000 times, as can be seen 55 ± 2
oWhole strip section structure is even later on for removal alloying in the 5wt.% HCl solution of C, illustrate that the strip section lives through identical removal alloying process, Fig. 2 b) is the SEM photo under amplifying 30000 times, can see uniform three-dimensional successive nano-porous structure, through adding up to such an extent that average skeleton is of a size of 121 ± 21 nm; Fig. 2 c) for the SEM photo under amplifying 3000 times, as can be seen 72 ± 2
oWhole strip section structure after the 5wt.% HCl solution interalloyization of C is even, illustrate that the strip section lives through identical removal alloying process equally, Fig. 2 d) is the SEM photo under amplifying 33000 times, can see uniform three-dimensional successive nano-porous structure, through adding up to such an extent that average skeleton is of a size of 152 ± 38 nm; Fig. 2 e) for the SEM photo under amplifying 2000 times, as can be seen 98 ± 2
oWhole strip section structure after the 5wt.% HCl solution interalloyization of C is even, illustrate that the strip section lives through identical removal alloying process equally, Fig. 2 f) is the SEM photo under amplifying 30000 times, can see uniform three-dimensional successive nano-porous structure, through adding up to such an extent that average skeleton is of a size of 210 ± 39 nm.
Fig. 3 is that the present invention is with 10
-5M CV is a probe molecule, be that substrate is immersed in the CV aqueous solution 2 hours with the nano porous metal, the surface enhanced Raman scattering spectrogram that obtains after the drying, the NPS sample that has three kinds of diverse microcosmic structures as can be seen all has the Raman scattering reinforcing effect for CV during as substrate, when skeleton was of a size of 152 ± 38 nm, reinforced effects was the most remarkable.
Embodiment
The present invention is described in detail below in conjunction with embodiment:
Embodiment one:Concrete steps are as follows:
A. it is long the Al-25at.%Ag alloy thin band to be cut into 2-3cm, gets 4-6 bar strip;
B. dispose 5wt.% HCl solution and place 3 beakers, strip is put into the HCl solution that configures, respectively 3 beakers are begun heating by room temperature simultaneously;
C. respectively three beakers are heated to 55 ± 2
oC, 72 ± 2
oC, 98 ± 2
oThe C insulation;
D. observe the bubble situation of Al element and HCl solution reaction in the container, wait not have obvious visible bubble in bubble, stop to be incubated, with strip by taking out in the HCl solution;
E. will wash 3-5 time with raw spirit through 3 alloy thin bands of a, b, c, d step, use deionized water rinsing 3-5 time subsequently;
F. dispose 10
-5The CV solution of M soaks nano porous metal 2 hours in the CV aqueous solution, and the back is taken out and washed repeatedly with distilled water, carries out the Raman scattering spectrum after the drying and detects.
Two kinds of NPS strips with Al-25 at.%Ag virgin alloy strip in the present embodiment and removal alloying acquisition, by X-ray diffractometer (X-ray Diffractomer, XRD) carry out material phase analysis, judge before the removal alloying and the removal alloying thing phase composite of strip later on.
Fig. 1 in the present embodiment in the visible accompanying drawing of material phase analysis result of related Al-25 at.%Ag alloy thin band and three kinds of NPS strips under differing temps, obtaining behind the removal alloying.Get Al-25at.% Ag virgin alloy strip by sosoloid α-Al (Ag) and intermetallic compound Ag according to Fig. 1
2Al two phase composites, through the removal alloying process under three temperature in HCl solution, only there is single face-centered cubic (f.c.c.) Ag phase in alloy thin band, illustrate that Al-25 at.%Ag alloy thin band all experiences identical removal alloying process at the electrolyte solution of differing temps, sosoloid α-Al (Ag) and intermetallic compound Ag in the alloy
2Al in the Al two-phase all is removed, only remaining single Ag phase.
With two kinds of NPS strips that obtain in the present embodiment, (Scanning Electron Microscope SEM) observes section structure, and records the skeleton size of two NPS respectively by scanning electronic microscope.
Fig. 2 in the visible accompanying drawing of NPS strip section structure pattern that obtains under three temperature in the present embodiment.Wherein Fig. 2 a) and b) be 55 ± 2
oThe section SEM photo of NPS behind the removal alloying in the 5wt.% HCl solution of C, Fig. 2 a) is the SEM photo under amplifying 3000 times, whole as can be seen strip section structure is even, illustrate that the strip section lives through identical removal alloying process, Fig. 2 b) is the SEM photo under amplifying 30000 times, can see uniform three-dimensional successive nano-porous structure, through adding up to such an extent that average skeleton is of a size of 121 ± 21 nm; Fig. 2 c) and d) be 72 ± 2
oThe SEM photo of NPS after the 5wt.% HCl solution interalloyization of C, Fig. 2 c) is the SEM photo under amplifying 3000 times, whole as can be seen strip section structure is even, illustrate that the strip section has experienced identical removal alloying process equally, Fig. 2 d) is the SEM photo under amplifying 33000 times, can see uniform three-dimensional successive nano-porous structure, through adding up to such an extent that average skeleton is of a size of 152 ± 38 nm; Fig. 2 e) and f) be 98 ± 2
oThe SEM photo of NPS after the 5wt.% HCl solution interalloyization of C, Fig. 2 e) is the SEM photo under amplifying 2000 times, whole as can be seen strip section structure is even, illustrate that the strip section lives through identical removal alloying process equally, Fig. 2 f) is the SEM photo under amplifying 30000 times, can see uniform three-dimensional successive nano-porous structure, through adding up to such an extent that average skeleton is of a size of 210 ± 39 nm.
With three kinds of NPS strips that have different size nanoporous microtexture obtaining under three kinds of temperature in the present embodiment 10
-5Soaked two hours in the M CV solution, behind the cleaning-drying, detect the Raman scattering active of NPS by laser capture microdissection Raman spectrometer (Renishaw inVia plus laser Raman spectrometer).
Fig. 3 in the present embodiment in the visible accompanying drawing of surface enhanced Raman scattering spectrogram of the NPS of three diverse microcosmic structures.Can see when using 10
-5The CV solution of M obtains strong Raman enhancing signal as the probe atomic time in the NPS substrate, the relative intensity at peak reaches 10
5The order of magnitude, and along with the difference of NPS microtexture size, the Raman reinforced effects is also variant, when the skeleton in the nano-porous structure on average was of a size of 152 ± 38 nm, the Raman reinforced effects was the most obvious.The electromagnetic coupled that this explanation size exists in concentrating between the interior skeleton of getting in touch each other of 152 ± 38 nm scopes is the most obvious for the reinforcing effect of Raman spectrum.
Claims (4)
1. one kind has the removal alloying preparation method that Raman strengthens the active nano porous metal substrate of scattering, it is characterized in that having following processing step:
A. it is long to be cut into 2-3cm with AB (C) alloy thin band that single roller revolves the method preparation of quenching; AB (C) alloy is a kind of among Al-Au, Al-Ag, Al-Cu, Mg-Ag, the Mg-Ag-Pd;
B. strip is put into container, electrolyte solution is housed in the container, container begins to be heated by room temperature simultaneously; Described electrolyte solution is the aqueous hydrochloric acid of 5wt.%;
C. container is heated to differing temps and insulation respectively;
D. observe the bubble situation of active metal and electrolyte solution reaction in the container, wait not have obvious visible bubble in bubble, stop to be incubated, with alloy thin band by taking out in the electrolyte solution;
E. will wash 3-5 time with raw spirit through the alloy thin band of a, b, c, d step, use deionized water rinsing 3-5 time subsequently; The nanoporous precious metal that obtains in AB (C) alloy is: nano-porous gold or nano-porous silver or nano porous palladium;
F. dispose the probe molecule of rare organic solution, take out base material is soaked 2h in probe molecule solution after, dry after washing repeatedly with distilled water as Raman test.
2. has the removal alloying preparation method that Raman strengthens the active nano porous metal substrate of scattering according to claim 1, it is characterized in that between the alloying element or the alloy constituent element between have difference in Electrode Potential, and a kind of element is wherein arranged is the precious metal element with Raman reinforcing effect.
3. reduce the removal alloying preparation method of nano-porous structure skeleton size significantly according to claim 1, it is characterized in that described electrolyte solution can dissolve more active element or constituent element in the alloy system, and do not influence the solution of precious metal element or torpescence constituent element.
4. reduce the removal alloying preparation method of nano-porous structure skeleton size significantly according to claim 1, it is characterized in that described electrolyte solution is a kind of in hydrochloric acid, sulfuric acid, oxalic acid, the phosphoric acid dilute solution, perhaps is a kind of in sodium hydroxide, the potassium hydroxide dilute solution.
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Cited By (9)
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| CN103255441A (en) * | 2013-05-20 | 2013-08-21 | 北京科技大学 | Method for preparing nano porous silver based on Ag-based amorphous alloy |
| CN103389296A (en) * | 2013-08-07 | 2013-11-13 | 苏州扬清芯片科技有限公司 | Quick preparation method of SERS (surface-enhanced Raman scattering) active substrate with three-dimensional nano porous structure |
| CN105112897A (en) * | 2015-09-08 | 2015-12-02 | 山东省医学科学院基础医学研究所 | Preparation method for porous copper-gold composite nanometer film material |
| CN106636717A (en) * | 2016-12-29 | 2017-05-10 | 天津理工大学 | Method for purifying nano-porous metal by evaporation differences |
| CN108169209A (en) * | 2018-01-22 | 2018-06-15 | 嘉兴长维新材料科技有限公司 | A kind of in-situ surface enhances Raman detection method |
| CN108613961A (en) * | 2018-04-20 | 2018-10-02 | 山东师范大学 | It is a kind of three-dimensional high sensitivity, the Raman active substrate of anti-friction |
| CN108971512A (en) * | 2018-09-14 | 2018-12-11 | 江西科技师范大学 | A kind of the green preparation and its application of the rectangular particle of porous spongy Ag |
| CN109524434A (en) * | 2017-09-20 | 2019-03-26 | 上海和辉光电有限公司 | A kind of back patch material structure, preparation method and its flexible display panels |
| RU2757750C1 (en) * | 2020-12-23 | 2021-10-21 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Electrochemical method for producing nanofibers of metallic copper |
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Cited By (12)
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| CN103255441A (en) * | 2013-05-20 | 2013-08-21 | 北京科技大学 | Method for preparing nano porous silver based on Ag-based amorphous alloy |
| CN103255441B (en) * | 2013-05-20 | 2015-06-10 | 北京科技大学 | Method for preparing nano porous silver based on Ag-based amorphous alloy |
| CN103389296A (en) * | 2013-08-07 | 2013-11-13 | 苏州扬清芯片科技有限公司 | Quick preparation method of SERS (surface-enhanced Raman scattering) active substrate with three-dimensional nano porous structure |
| CN105112897A (en) * | 2015-09-08 | 2015-12-02 | 山东省医学科学院基础医学研究所 | Preparation method for porous copper-gold composite nanometer film material |
| CN106636717A (en) * | 2016-12-29 | 2017-05-10 | 天津理工大学 | Method for purifying nano-porous metal by evaporation differences |
| CN109524434A (en) * | 2017-09-20 | 2019-03-26 | 上海和辉光电有限公司 | A kind of back patch material structure, preparation method and its flexible display panels |
| CN108169209A (en) * | 2018-01-22 | 2018-06-15 | 嘉兴长维新材料科技有限公司 | A kind of in-situ surface enhances Raman detection method |
| CN108169209B (en) * | 2018-01-22 | 2021-02-02 | 嘉兴长维新材料科技有限公司 | In-situ surface enhanced Raman detection method |
| CN108613961A (en) * | 2018-04-20 | 2018-10-02 | 山东师范大学 | It is a kind of three-dimensional high sensitivity, the Raman active substrate of anti-friction |
| CN108971512A (en) * | 2018-09-14 | 2018-12-11 | 江西科技师范大学 | A kind of the green preparation and its application of the rectangular particle of porous spongy Ag |
| CN108971512B (en) * | 2018-09-14 | 2021-04-02 | 江西科技师范大学 | Green preparation method and application of porous spongy Ag square particles |
| RU2757750C1 (en) * | 2020-12-23 | 2021-10-21 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Electrochemical method for producing nanofibers of metallic copper |
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