CN105277525A - BN sub-nano chamber-based super strong SERS substrate and preparation method - Google Patents
BN sub-nano chamber-based super strong SERS substrate and preparation method Download PDFInfo
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Abstract
The present invention discloses a BN sub-nano chamber-based super strong SERS substrate and a preparation method, and compared with the prior art, the BN sub-nano chamber-based super strong SERS substrate has good sensitivity, strong oxidation resistance, low cost, long life, and good reproducibility, and the preparation process is simple, time-saving and controllable. A strong Raman spectroscopy detection signal still can be obtained after calcinations of the substrate in the air at a certain temperature, and compared with the prior art, the BN sub-nano chamber-based super strong SERS substrate has superior stability. The BN is easy and fast to ultrasonically peel by a probe. Furthermore, BN nanosheets peeled by the probe method are thin, and are in favor of acquisition of the strong Raman spectroscopy detection signal in the constructed substrate; and by the method of direct spin coating of an Au film, complex steps of production of BN grown by traditional transfer CVD method can be eliminated, and the cost is greatly reduced. The substrate provides technical supports for further promotion of promotion and application of SERS technology.
Description
Technical field
The invention belongs to detection technique field, particularly relate to a kind of superpower SERS substrate based on the sub-nano-cavity of BN and preparation method thereof.
Background technology
As a kind of harmless, contactless and can realize the spectral analysis technique that molecular level detects with testing molecule, Surface enhanced raman spectroscopy (SERS) is widely used in fields such as environment, biology, chemistry.But, at present, obtain the developing direction that stronger SERS signal and more stable SERS substrate are still this technology.Improving SRES signal from the difform metal of initial synthesis (gold, silver etc.) nano particle, obtaining Sensitive Detection to recently constructing different structure (Metal/grapheme, metal/molybdenum sulfide etc.), SERS technology experienced by the evolution (Adv.Mater. of long period, 2010,22 (37): 4136-4139, Nanoscale, 2010,2,2733-2738, NanoLett.2014,14,5329-5334).But because sensitivity is not high, the deficiency such as repeatable and poor stability, these SERS substrates are still not suitable for large-scale application.
At present, in order to obtain stronger SERS signal, researcher has constructed Metal/grapheme/metal sandwich structure, thus obtains double plasma enhancing effect (Chem.Commun., 2015,51,866-869).In sandwich structure, the selection of constructing sub-nano-cavity material is most important.Although said structure obtains larger enhancing SERS signal, but due to the aerial thermal stability of Graphene and the shortcoming such as inoxidizability is poor, jump operation is complicated, above-mentioned SERS substrate still can not be used widely.
Summary of the invention
The technical issues that need to address of the present invention are: the object of this invention is to provide a kind of superpower SERS substrate based on the sub-nano-cavity of BN and preparation method thereof.The present invention constructs gold nano grain/boron nitride/golden film (AuNPs/BN/Aufilm) sandwich structure SERS substrate.The construction material of sub-nano-cavity selects BN, not only Au nano particle and Au film can be separated and produce superpower plasmon coupling effect, thus obtain superpower SERS enhancing signal, and due to the thermal stability of boron nitride superelevation and inoxidizability (room temperature coefficient of heat conductivity ~ 400W/m/K, 5 times of Graphene), this substrate has higher stability.In addition, preparing of BN nanometer sheet adopts commercially available hexagonal boron nitride method with probe sonication in water, the boron nitride prepared is spin-coated on Au film, simply, fast, not only eliminate the complicated transfer process of the BN of chemical vapor deposition (CVD) method growth, and greatly reduce cost.Due to advantages such as superpower sensitivity, higher stability, shirtsleeve operation step and lower costs, this substrate can advance SERS technology in the widespread use of different field further.
Technical scheme of the present invention is: design a kind of superpower SERS substrate based on the sub-nano-cavity of BN, it is characterized in that, described SERS substrate is three-decker, and upper strata is metal nanoparticle, and middle layer is BN, and lower floor is metal film.
The further technical scheme of the present invention is: described metal nanoparticle is Au nano particle.
The further technical scheme of the present invention is: described metal film is Au film.
The further technical scheme of the present invention is: SERS substrate also comprises the adhesion layer structure for fixing lower metal film, and adhesion layer structure comprises Si sheet and Cr; Wherein Cr is positioned on Si sheet; Metal film is positioned on Cr.
The further technical scheme of the present invention is: a kind of preparation method of the superpower SERS substrate based on the sub-nano-cavity of BN, comprises the steps:
Step one: evaporation one deck Cr on Si sheet, as the adhesion layer of described substrate;
Step 2: evaporation layer of Au film on the Cr in adhesion layer;
Step 3: the preparation of BN/Au membrane structure, comprises following sub-step:
Sub-step 1: BN is added in deionized water, ultrasonic process 8-10 hour;
Sub-step 2: pour out after the solution after ultrasonic process being poured into the centrifugal 20-25 of centrifuge tube minute, obtain BN nanometer sheet;
Sub-step 3: BN nanometer sheet be coated on the Au in step 2, forms BN/Au membrane structure;
Step 3:: by Au particle evaporation on the BN described in step 2, form Au/BN/Au membrane structure.
The further technical scheme of the present invention is: on Si sheet with
speed evaporation last layer thickness be the Cr of 2-5 nanometer.
The further technical scheme of the present invention is: on Cr with
speed evaporation last layer thickness be the Au film of 100 nanometers.
The further technical scheme of the present invention is: added by 20-40mgBN in 200ml deionized water.
The further technical scheme of the present invention is: BN nanometer sheet be spin-coated on Au film with the speed of 1500-2000 rev/min.
The further technical scheme of the present invention is: in BN nanometer sheet with
speed evaporation last layer thickness be the Au nano particle of 20 nanometers.
Invention effect
Technique effect of the present invention is: compared with prior art, and the SERS substrate sensitivity of the sub-nano-cavity of BN provided by the invention is good, and not only inoxidizability is strong, and with low cost, and the life-span is long, reproducible, and preparation process is simple and easy, saves time, controlled.This substrate, in atmosphere still can obtain stronger Raman spectrum detection signal after certain temperature calcination, compared with existing substrate, has superpower stability.Probe sonication is adopted to peel off BN convenient, fast.In addition, the BN nanometer sheet peeled off by sonde method is thinner, is conducive to obtaining stronger Raman spectrum detection signal in the substrate of constructing.Moreover, by being directly spun on method on Au film, eliminating the complex steps of the BN of tradition transfer CVD growth, also greatly reducing cost simultaneously.This substrate is that the promotion and application promoting SERS technology further provide technical support.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of BN, and arrow represents the grating constant of BN, and other are scale.
Fig. 2 is the raman spectrum strength of Au nano particle/BN/Au film substrate to the detection of rhodamine after different temperatures calcining.Horizontal ordinate is wave number, and ordinate is intensity.
Embodiment
Below in conjunction with concrete embodiment, technical solution of the present invention is further illustrated.
Based on a superpower SERS substrate for the sub-nano-cavity of BN, it is characterized in that, described SERS substrate is three-decker, and upper strata is metal nanoparticle, and middle layer is BN, and lower floor is metal film.In the present embodiment,
Metal nanoparticle is Au nano particle.Metal film is Au film.SERS substrate also comprises the adhesion layer structure for fixing lower metal film, and in the present embodiment, adhesion layer structure comprises Si sheet and Cr; Wherein Cr is positioned on Si sheet; Metal film is positioned on Cr.
The present invention also provides a kind of superpower SERS substrate based on the sub-nano-cavity of BN and preparation method thereof, prepares primarily of following steps:
Step 1, the preparation of Au film and the adhesion layer for fixing Au film: on the silicon chip of wash clean with
namely the speed evaporation last layer thickness of 1 nanometer per second is that the chromium of 2-5 nanometer is as adhesion layer.Be the Au film of 100 nanometers with same speed evaporation last layer thickness in layers of chrome afterwards.
Step 2, the preparation of BN nanometer sheet: take the commercially available BN of 20-40mg and add in 200ml deionized water.By above-mentioned solution probe sonication 8-10 hour.Solution after ultrasonic to pour in centrifuge tube centrifugal 20-25 minute under the condition of 6000 revs/min into.Centrifugal good solution is derived and namely obtains BN nanometer sheet.
Step 3, the preparation of BN/Au membrane structure: the solution after centrifugal is poured out and uses spin coating instrument with on the speed spin coating of 1500-2000 rev/min Au film in step 1.Namely BN/Au membrane structure is obtained after drying.
Step 4, the preparation of Au nano particle/BN/Au membrane structure: in step 3 on BN with
speed evaporation last layer thickness be that namely the Au particle of 20 nanometers obtains Au nano particle/BN/Au membrane structure.
It should be noted that, ultrasonic effect is peeled off, all the BN added can not be peeled off due to ultrasonic, so centrifugal, what after centrifugal, those were not stripped or peeled off is not that very thin BN will be deposited on centrifugal tube wall, and the thinner BN peeled off just is dissolved in water, pours out after centrifugal and namely obtain required BN.Because Au nano particle/BN/Au film is very thin, naked eyes be can't see substantially, so will to be put on a supporter such as silicon chip here, adhesion layer conveniently fixes Au film.)
Substrate being applied as in practice: drip 3-8 in Au nano particle/BN/Au membrane structure substrate and drip rhodamine liquor and dry, detect under afterwards they being placed on Raman spectrometer.The condition that spectrometer is selected is 50X times of mirror and 633 nanometer laser wavelength, and laser energy selects 0.5%.After Au nano particle/BN/Au film sandwich structure substrate is calcined 2-5 minute in atmosphere with 100-400 degree Celsius, repeat above-mentioned steps, continue calcining.
It should be noted that, calcining is the favorable repeatability in order to verify this substrate, and after calcining, the rhodamine of first time detection has just been calcined not, and substrate does not change.Again detect after calcining, be the good stability in order to substrate is described, still can use after namely at high temperature having calcined, other substrates existing can not be calcined like this, this substrate also illustrating in the present invention can be used in comparatively in rugged environment, the place that such as temperature is higher.)
The present invention also provides a kind of superpower SERS substrate based on the sub-nano-cavity of BN and preparation method thereof.Metal in substrate can also be silver, copper etc.Moreover, bottom metal can be film also can be nano particle, i.e. metal nanoparticle/BN/ metal nanoparticle, metal nanoparticle/BN/ metal film.
Embodiment one:
The silicon chip acetone of 3.5cm × 3.5cm cleans up and dries.With
speed to mix the chromium film of evaporation last layer 2nm on silicon chip.Again with same speed evaporation layer of Au film on chromium film.Take the commercially available BN of 20mg to add in 200ml deionized water and with probe sonication 8 hours.Solution after ultrasonic to be poured in centrifuge tube under the condition of 6000 revs/min centrifugal 20 minutes.Solution after centrifugal is poured out and uses spin coating instrument to be spin-coated on above-mentioned Au film with the speed of 1500 revs/min and to dry.On BN with
speed evaporation last layer thickness be the Au particle of 20 nanometers.Rhodamine being configured to concentration is 10-6mol/L solution.Au nano particle drips 5 rhodamine liquor configured and dries.Substrate with rhodamine is detected under Raman spectrometer.It is 1.9 × 106 that result display improves the factor (EF) value.By the sandwich structure on silicon chip in atmosphere with 100 degrees Celsius of calcinings 5 minutes.Result display EF is 1.8 × 106.
Embodiment two:
The silicon chip acetone of 3cm × 3cm cleans up and dries.With
speed to mix the chromium film of evaporation last layer 3nm on silicon chip.Again with same speed evaporation layer of Au film on chromium film.Take the commercially available BN of 30mg to add in 200ml deionized water and with probe sonication 8 hours.Solution after ultrasonic to be poured in centrifuge tube under the condition of 6000 revs/min centrifugal 25 minutes.Solution after centrifugal is poured out and uses spin coating instrument to be spin-coated on above-mentioned Au film with the speed of 2000 revs/min and to dry.On BN with
speed evaporation last layer thickness be the Au particle of 20 nanometers.Rhodamine being configured to concentration is 10-6mol/L solution.Au nano particle drips 5 rhodamine liquor configured and dries.Substrate with rhodamine is detected under Raman spectrometer.Result display EF value is 1.4 × 106.By the sandwich structure on silicon chip in atmosphere with 300 degrees Celsius of calcinings 3 minutes.Result display EF is 1.2 × 106.
Embodiment three:
The silicon chip acetone of 3cm × 3cm cleans up and dries.With
speed to mix the chromium film of evaporation last layer 5nm on silicon chip.Again with same speed evaporation layer of Au film on chromium film.Take the commercially available BN of 40mg to add in 200ml deionized water and with probe sonication 10 hours.Solution after ultrasonic to be poured in centrifuge tube under the condition of 6000 revs/min centrifugal 20 minutes.Solution after centrifugal is poured out and uses spin coating instrument to be spin-coated on above-mentioned Au film with the speed of 1600 revs/min and to dry.On BN with
speed evaporation last layer thickness be the Au particle of 20 nanometers.Rhodamine being configured to concentration is 10-6mol/L solution.Au nano particle drips 5 rhodamine liquor configured and dries.Substrate with rhodamine is detected under Raman spectrometer.Result display EF value is 1.8 × 106.By the sandwich structure on silicon chip in atmosphere with 300 degrees Celsius of calcinings 2 minutes.Result display EF is 1.5 × 106.
Embodiment four:
The silicon chip acetone of 4cm × 4cm cleans up and dries.With
speed to mix the chromium film of evaporation last layer 5nm on silicon chip.Again with same speed evaporation layer of Au film on chromium film.Take the commercially available BN of 40mg to add in 200ml deionized water and with probe sonication 9 hours.Solution after ultrasonic to be poured in centrifuge tube under the condition of 6000 revs/min centrifugal 20 minutes.Solution after centrifugal is poured out and uses spin coating instrument to be spin-coated on above-mentioned Au film with the speed of 1700 revs/min and to dry.On BN with
speed evaporation last layer thickness be the Au particle of 20 nanometers.Rhodamine being configured to concentration is 10-6mol/L solution.Au nano particle drips 5 rhodamine liquor configured and dries.Substrate with rhodamine is detected under Raman spectrometer.Result display EF value is 1.5 × 106.By the sandwich structure on silicon chip in atmosphere with 200 degrees Celsius of calcinings 2 minutes.Result display EF is 1.8 × 106.
The BN nanometer sheet of the ultrasonic acquisition of sonde method is ultra-thin, and the substrate being conducive to constructing obtains stronger signal, see Fig. 1.Respectively 100,200,300, detect rhodamine at this after 400 degrees Celsius of calcined substrate and still can obtain stronger detection signal.The superpower stability of substrate is described, see Fig. 2.
Substrate in the present invention is to obtain stronger Raman spectrum detection signal, and strengthening signal is to detect some specific composition, such as drugs, explosive, virus.If noxious material low dose is added, common detection means is easy to just can detect, and a small amount of interpolation is just not easy to detect, and the substrate described in the present invention can detect, such as, noxious material is dissolved in water and stirs evenly, drop in substrate afterwards and get on to survey Raman, just can measure the coherent signal of noxious material easily.Calcining substrate in the present embodiment, is that this is the advantage that other substrates do not have in order to illustrate that our substrate has good stability, also illustrate that our substrate can be used in some conditions and compare in rugged environment simultaneously.
Although content of the present invention has done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple amendment of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1., based on a superpower SERS substrate for the sub-nano-cavity of BN, it is characterized in that, described SERS substrate is three-decker, and upper strata is metal nanoparticle, and middle layer is BN, and lower floor is metal film.
2. a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 1, it is characterized in that, described metal nanoparticle is Au nano particle.
3. a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 1, it is characterized in that, described metal film is Au film.
4. a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 1, it is characterized in that, SERS substrate also comprises the adhesion layer structure for fixing lower metal film, and adhesion layer structure comprises Si sheet and Cr; Wherein Cr is positioned on Si sheet; Metal film is positioned on Cr.
5., based on a preparation method for the superpower SERS substrate of the sub-nano-cavity of BN, comprise the steps:
Step one: evaporation one deck Cr on Si sheet, as the adhesion layer of described substrate;
Step 2: evaporation layer of Au film on the Cr in adhesion layer;
Step 3: the preparation of BN/Au membrane structure, comprises following sub-step:
Sub-step 1: BN is added in deionized water, ultrasonic process 8-10 hour;
Sub-step 2: pour out after the solution after ultrasonic process being poured into the centrifugal 20-25 of centrifuge tube minute, obtain BN nanometer sheet;
Sub-step 3: BN nanometer sheet be coated on the Au in step 2, forms BN/Au membrane structure;
Step 3:: by Au particle evaporation on the BN described in step 2, form Au/BN/Au membrane structure.
6. the preparation method of a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 5, is characterized in that, on Si sheet with
speed evaporation last layer thickness be the Cr of 2-5 nanometer.
7. the preparation method of a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 5, is characterized in that, on Cr with
speed evaporation last layer thickness be the Au film of 100 nanometers.
8. the preparation method of a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 5, is characterized in that, added by 20-40mgBN in 200ml deionized water.
9. the preparation method of a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 5, is characterized in that, BN nanometer sheet be spin-coated on Au film with the speed of 1500-2000 rev/min.
10. the preparation method of a kind of superpower SERS substrate based on the sub-nano-cavity of BN as claimed in claim 5, is characterized in that, in BN nanometer sheet with
speed evaporation last layer thickness be the Au nano particle of 20 nanometers.
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| CN110441283A (en) * | 2019-07-22 | 2019-11-12 | 浙江大学 | A kind of novel telluride gallium-terminated surface enhancing Raman substrate and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103203462A (en) * | 2013-03-21 | 2013-07-17 | 上海大学 | Preparation method of boron nitride nanosheet-silver nanoparticle composite material |
| CN103774113A (en) * | 2014-02-24 | 2014-05-07 | 中国科学院上海微系统与信息技术研究所 | Method for preparing hexagonal boron nitride film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103203462A (en) * | 2013-03-21 | 2013-07-17 | 上海大学 | Preparation method of boron nitride nanosheet-silver nanoparticle composite material |
| CN103774113A (en) * | 2014-02-24 | 2014-05-07 | 中国科学院上海微系统与信息技术研究所 | Method for preparing hexagonal boron nitride film |
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| CN110441283A (en) * | 2019-07-22 | 2019-11-12 | 浙江大学 | A kind of novel telluride gallium-terminated surface enhancing Raman substrate and preparation method thereof |
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