CN107101967A - A kind of application ITO nano materials as infrared spectrum sum of fundamental frequencies area surface enhanced substrate method - Google Patents
A kind of application ITO nano materials as infrared spectrum sum of fundamental frequencies area surface enhanced substrate method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 45
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 33
- 239000000523 sample Substances 0.000 claims abstract description 78
- 239000002105 nanoparticle Substances 0.000 claims abstract description 53
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- 238000003786 synthesis reaction Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 28
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 16
- 239000010409 thin film Substances 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- FHTDDANQIMVWKZ-UHFFFAOYSA-N 1h-pyridine-4-thione Chemical compound SC1=CC=NC=C1 FHTDDANQIMVWKZ-UHFFFAOYSA-N 0.000 claims description 10
- FHNINJWBTRXEBC-UHFFFAOYSA-N Sudan III Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 FHNINJWBTRXEBC-UHFFFAOYSA-N 0.000 claims description 10
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- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 239000007983 Tris buffer Substances 0.000 claims description 4
- 150000001805 chlorine compounds Chemical class 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 4
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 4
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- 239000010408 film Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
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- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- CMNQZZPAVNBESS-UHFFFAOYSA-N 6-sulfanylhexanoic acid Chemical class OC(=O)CCCCCS CMNQZZPAVNBESS-UHFFFAOYSA-N 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims description 2
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
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- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 2
- 229940043267 rhodamine b Drugs 0.000 claims description 2
- 238000001338 self-assembly Methods 0.000 claims description 2
- NBOMNTLFRHMDEZ-UHFFFAOYSA-N thiosalicylic acid Chemical compound OC(=O)C1=CC=CC=C1S NBOMNTLFRHMDEZ-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- IQDGSYLLQPDQDV-UHFFFAOYSA-N dimethylazanium;chloride Chemical compound Cl.CNC IQDGSYLLQPDQDV-UHFFFAOYSA-N 0.000 claims 1
- 239000005357 flat glass Substances 0.000 claims 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims 1
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- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 description 2
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 description 2
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 2
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- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B82—NANOTECHNOLOGY
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
A kind of application ITO nano materials as infrared spectrum sum of fundamental frequencies area surface enhanced substrate method, belong to nanometer technology and field of new materials, specifically related to one kind carries out the innovative approach of surface enhanced near-infrared (SENIR) and surface-enhanced infrared spectroscopy (SEIRAS) detection to probe molecule with semiconductor nano material or film oxidation indium tin (ITO) for substrate in infrared spectrum sum of fundamental frequencies area (0.7~7.7 μm of wave-length coverage).Synthesis including plasmon resonance nano material ITO, probe molecule surface modification prepare, carry out three parts of SENIR and SEIRAS detections to probe molecule by new SENIR and SEIRAS substrates of ITO nano-particles, film or sol material.By strengthening the use of substrate, SENIR the and SEIRAS signals that detection is adsorbed onto ITO nano-material surfaces are remarkably reinforced than the sum of fundamental frequencies area infrared signal of probe molecule body, and enhancer can reach 104.This method has widened the range of choice of base material for the research of SEIRAS effects；It is a brand-new expansion to infrared spectrum detection function.
Description
Technical field
The invention belongs to nanometer technology and field of new materials, and in particular to one kind is with semiconductor nano material or film oxidation
Indium tin (Indium Tin Oxide, ITO) is substrate, in infrared spectrum sum of fundamental frequencies area (0.7~7.7 μm of wave-length coverage) to probe point
Son carries out surface enhanced near-infrared (Surface-enhanced near infrared, SENIR) and surface enhanced infrared absorption
The innovative approach of spectrum (Surface-enhanced infrared absorption spectroscopy, SEIRAS) detection
With application.
Background technology
1980, Hartstein etc. was using total internal reflection technique study sputtering island silver on a silicon substrate, gold thin film
Surface-enhanced infrared spectroscopy (SEIRAS) phenomenon is found that first during to paranitrobenzoic acid (PNBA) equimolecular absorption.
Then, the presence that this is tested and confirms SEIRAS is repeated in Hatta et al..This discovery opens the infrared suction of surface enhanced
The research field of receipts.
Infrared absorption spectroscopy is the vibrational spectrum of molecule, and it mainly studies the chemical combination changed in vibration with dipole moment
Thing, its structural information is understood according to features such as the wavelength of their infrared absorption bands, intensity and shapes, therefore infrared absorption spectroscopy exists
Compound structure is identified and to analyze context of detection significant and be extremely widely applied.Compared to common infrared absorption
Spectrum, the spectral intensity of SEIRAS technologies can improve tens times, so as to obtain, sensitivity is higher, the more preferable signal of signal to noise ratio.
SEIRAS is the supplement to conventional infrared absorption spectroscopy, even more huge to improve.
Substrate used in current SEIRAS is mainly noble silver or gold, and they can be by the infrared absorption of probe molecule
Signal improves tens times.But noble metal is expensive, it is unfavorable for being widely popularized.Although some transition metal also have SEIRAS letters
Number, but the research for transition metal is also seldom, do not know for sure their surface enhanced infrared absorption effect.Will
SEIRAS effects widen other materials and do not obtain the progress that tool has significant practical applications also.
In addition, existing research shows, it is known that SEIRAS substrates there is obvious increasing in 7.7~25 μm of wave-length coverage
Potent fruit, this interval is mainly mid-infrared spectral fingerprint region.And to contain wavelength wide from 0.7 to 1000 μm for infrared spectrum
General spectrum range, with very discrete Energy distribution, the material intrinsic properties of noble silver or gold causes them can not possibly be
It is extensive interval with enhancing effect.In 0.7~7.7 μ m wavelength range, i.e. infrared spectrum sum of fundamental frequencies area, surface enhanced substrate
So far do not report.Therefore, surface enhanced substrate of the exploitation in infrared spectrum sum of fundamental frequencies area is a challenge.
Mainly corresponding in 0.7 to 7.7 μm of wave-length coverages is infrared spectrum sum of fundamental frequencies area, includes part middle infrared spectral region
(2.5~7.7 μm of wave-length coverage) and whole near infrared spectrum (0.7~2.5 μm of wave-length coverage).The sum of fundamental frequencies area of infrared spectrum is special
To levy peak be the uptake zone that hydric group (O-H, N-H, C-H) vibrates in organic molecule, by the sum of fundamental frequencies area wave band for scanning sample
Infrared spectrum, can obtain the characteristic information of organic molecule hydric group in sample.It is convenient, fast that the spectrum analysis in sum of fundamental frequencies area has
Speed, efficient, accurate and cost are relatively low, do not destroy sample, chemical reagent are not consumed, the advantages of free from environmental pollution.Infrared spectrum
Fingerprint region characteristic peak it is main it is corresponding be the stretching vibration of various singly-bounds and the flexural vibrations of most groups.Although it is to molecule
The susceptibility of structure change is high, but the oscillatory type in this region is complicated and overlapping, and characteristic is poor.Therefore, develop infrared
The surface enhanced substrate in spectrum sum of fundamental frequencies area is that one of infrared spectrum detection function is completely newly expanded.
Tin indium oxide (Indium Tin Oxide, ITO) is generally considered as the indium oxide of tin dope.Indium oxide is in itself
More preferable electric conductivity is provided with after a kind of semiconductor, doped tin.Research shows that ITO free electron is close during the doping of appropriate amount
Degree is maximum, resistivity is minimum.Doping excessively can not only be such that electronics is limited near tin atom, reduce free electronic concentration, can also
Carrier mobility is reduced because of scattering enhancing.Because band gap reduces, the transparency of material can also be affected.It is generally acknowledged that
Optimal doping is 10% or so.
The synthetic method of ITO nano materials is broadly divided into thin film deposition and solution synthesizes two kinds.Film forming method is mainly sharp
With gas evaporation, spray pyrolysis, pulsed laser deposition etc., these methods are difficult to control the size of ITO nano particles.Base
Include Penchini methods, coprecipitation method etc. in the synthesis of solution, many methods can only obtain In (OH)3Or InOOH forerunner
Body is, it is necessary to which oxide product could be obtained by further heating, and the use of surfactant will also result in it on ITO materials
Residual, influence material subsequent characterizations and the application in Surface-enhanced spectroscopic.To make material be more suitable for being used as surface enhanced
Substrate, the ITO materials of synthesis need the surface with uniform size, shape and cleaning.Based on as above considering, this selected works
Select tin atom in solvent process for thermosynthesizing, the method to offset from+4 valencys to oxidation state direction, oxygen atom is not simply yet
With In3+And Sn4+With reference to bonding, but there is complicated electronic migration.Mix the forbidden band of the ITO semi-conducting materials constituted after tin
Width is widened, at the same electric conductivity increase, carrier concentration improve, the combination of the two make ITO have excellent electric conductivity and
Surface enhanced characteristic.
The content of the invention
For above the problem of, we are carried out using ITO semi-conductor nano particles or thin-film material as substrate first
SENIR and SEIRAS detections.ITO high conductivity is a tin original as caused by the tin atom and the vacancy of oxygen atom that adulterate
Son doping enters indium oxide (In2O3) lattice when will provide for a free electron, therefore tin atom addition to improving carrier
Density has very great help.The 5s electronics of tin atom is stabilized under the energy of conduction band bottom, and Lacking oxygen is bielectron donor level,
The 5s electronics of tin atom is then single electron donor level.A small amount of tin atom is added in indium oxide, tin atom into alternate form impurity,
Sn4+Instead of In3+.As the Sn of high price4+When mixing indium oxide, Sn4+Occupy In3+Position, generate cation vacancy and oxygen and lack
Fall into, cause electrical type defect, at this moment the density of carrier is to influence the key factor of resistance.Therefore the ITO materials that we synthesize
Free electron density is big, resistivity is small, with infrared spectrum sum of fundamental frequencies area plasmon resonance characteristic, in visible region extinction coefficient
Very little.The scope of existing SEIRAS base materials had both been widened in the discovery of infrared spectrum sum of fundamental frequencies area plasmon resonance characteristic, more
The excitation wavelength of surface enhanced substrate is extended to infrared spectrum sum of fundamental frequencies area from traditional infrared spectrum fingerprint region, has surmounted existing
SEIRAS technologies.
It is an object of the invention to provide a kind of new SENIR and SEIRAS substrate Is TO.ITO, which has, high freely to be carried
Sub- concentration is flowed, the characteristic in terms of having surface plasma in infrared spectrum sum of fundamental frequencies area can be applied to surface enhanced effect
In.The present invention has widened the scope of SEIRAS substrates, is further while developing new wavelength scope of application SENIR substrates
The mechanism for studying SENIR and SEIRAS effects provides theoretical and experimental basis.The enhancer of new SENIR and SEIRAS substrates
Reach 104, may have extensive potential application in surface analysis science.
Method of the present invention includes infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis, probe
Molecular surface modification is prepared and using ITO nano-particles or thin-film material as new SENIR and SEIRAS substrates to probe point
Son carries out SENIR and SEIRAS and detects three parts.It is specific as follows：
(1) infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis：
(1) 0.1~2.5g Indium Tris acetylacetonate and 0.01~0.27g acetylacetone,2,4-pentanedione stannic chlorides is weighed；
(2) 10~20mL n-butanol, after stirring, ultrasound 10~20 minutes are added into above-mentioned sample；
(3) by step (2) resulting solution at 150~200 DEG C hydro-thermal reaction 30~60 hours, be cooled to after room temperature will production
Thing is centrifuged, and obtains solid product；
(4) solid product is alternately washed by ethanol, deionized water, then the freeze-day with constant temperature under 60~80 DEG C of vacuum conditions
10~20 hours, obtain ITO nanoparticle powders；
(5) by obtained ITO nanoparticle powders deionized water or organic solvent (ethanol, toluene, chloroform or hexamethylene
Alkane) dissolving, stir 4~8 hours, obtain the ITO nanoparticle sols that concentration is 0.1~8.5g/L.
(2) surface modification of probe molecule：
Weigh 0.01~0.1g of ITO nanoparticle powders that above-mentioned steps (4) obtain and be added to 10-10~10-2Mol/L's
In the aqueous solution or ethanol solution of probe molecule, stir 1~24 hour, be cleaned multiple times with probe molecule solutions identical solvent
And centrifugation, unadsorbed probe molecule is removed, is then dried naturally, obtaining surface modification there are the ITO nanometers of probe molecule
Particle powder；
Or, 10 that 5~1000 μ L above-mentioned steps (5) are obtained-10~10-2The aqueous solution or second of mol/L probe molecule
Alcoholic solution is added dropwise in 0.01~0.1g ITO nanoparticle powders, is then dried naturally, you can obtaining surface modification has probe
The ITO nanoparticle powders of molecule；
Or, ITO nano-particles are assembled into substrate by the method for self assembly, specific method is：First in glass
The silver or gold thin film of the μ m-thick of one layer of 10nm~4 is deposited on piece or silicon chip substrate under vacuum, is dipped the substrate into again after taking-up
10~30 minutes in 0.01~0.1mol/L diallyl dimethyl ammoniumchloride (PDDA) aqueous solution, deionization is used after taking-up
Water is cleaned, nitrogen drying；Then dip the substrate into again in ITO nanoparticle sols 4~8 hours, after taking-up with ITO nanoparticles
Sub- colloidal sol identical solvent is cleaned, nitrogen drying, and obtaining surface self-organization has the substrate of ITO nano-particles；Finally by base
Bottom is dipped into 10-10~10-2In the aqueous solution or ethanol solution of mol/L probe molecule, after 4~12 hours take out, with probe
Molecular solution identical solvent clean repeatedly, removes unadsorbed probe molecule, and nitrogen is dried up, and obtaining surface modification has spy
The ITO nanoparticulate thin films of pin molecule；
Or, it is directly added into 10 in obtained ITO nanoparticle sols-10~10-2Mol/L probe molecule it is water-soluble
Liquid or ethanol solution, are stirred 2~8 hours, you can obtaining surface modification has the ITO nanoparticle sols of probe molecule.
(3) carried out the ITO nano materials obtained above for being modified with probe molecule as SENIR and SEIRAS substrates
SENIR and SEIRAS tests：
The instrument that the present invention is used is Bruker Fourier Transform Infrared Spectrometer 80v
With Bruker Near infrared spectrometer MPA.
In the above method, SENIR and SEIRAS is carried out as substrate using ITO nano materials and tested, ITO nano materials can
To use the form of different forms, such as powder, film or colloidal sol.
(1) there are the ITO nanoparticle powder samples of probe molecule for surface modification, near infrared region can directly be tested, in
Infrared region is tested using KBr (KBr) tabletting method.Tested using pressing potassium bromide troche method, specific tabletting method is：1. it is first
First, 200mg KBr and 1~6mg institute's test sample product are taken, is ground 1~5 minute.Note along a direction grinding, so as not to it is broken
Bad crystal structure.Workbench should be equipped with infrared lamp, whole to be completed under infrared lamp baking.2. then, modulus has, wiped clean.
Base is installed, interior module smooth surface is put into upwards, is uniformly put into sample with medicine spoon, by fore-set plus well, can gently rotate and
Sample is set uniformly to spread out.3. mould is placed on tablet press machine, screws spiral, fasten vent valve, be forced into 20MPa, stop 1~4
Minute.4. it is last, vent valve is slowly opened, pressure is slowly declined to 0.Turn on spiral and take out mould.Base is opened, reversely pressure
Go out interior module, the tabletting pressed is carefully taken out with the medicine shovel of plane, is put into tablet folder.
(2) there are the ITO nanoparticulate thin films samples of probe molecule, near infrared region and middle infrared for surface modification
Directly test.
(3) there are the ITO nanoparticle sol samples of probe molecule for surface modification, can be by 10~1000 μ L colloidal sol
Drop on metallic reflection piece, wait it to dry, near infrared region is directly tested, middle infrared is tested using infrared sweep angle reflection accessory.
In the above method, SENIR and SEIRAS are carried out as substrate using ITO nano materials and detected, probe molecule can be with
For：Mercaptopropionic acid, 6- mercaptohexanoic acids, to mercaptobenzoic acid, pyridine, 4-Mercaptopyridine, rhodamine B, rhodamine 6G, acid red,
Tonyred etc..Probe molecule is that analysis is pure.
In the above method, SENIR and SEIRAS is carried out as substrate using ITO nano materials and detected, is as a result shown：ITO
Nano material has the optical characteristics of surface enhanced in infrared spectrum sum of fundamental frequencies area.
In the above method, infrared enhancing mechanism is：When the electronics of ITO conduction bands is consistent with the vibration frequency of incident light photons,
Plasmon resonance can be produced, strong absorption is produced to incident light, so as to produce surface enhanced near-infrared and surface enhanced is red
Outer absorbing phenomenon.
In the above method, SENIR and SEIRAS is carried out as substrate using ITO nano materials and detected, the results of FT-IR
It is preliminary to judge to draw with reference to SEM (SEM), x-ray photoelectron power spectrum (XPS) and transmission electron microscope (TEM)
The reason for playing signal enhancing is Electromagnetic enhancement, belongs to physics enhancing.
In the present invention, using ITO nano materials as substrate, infrared detection is carried out to probe molecule, further widened
Strengthen the mode of infrared test.By the use of new substrates, the letter that more probe molecules interact with substrate can be obtained
Breath, the mechanism for further research infrared spectrum provides experimental basis, while also turning into generally applicable for development infrared spectrum
Characterization tool lays the foundation.
We are found that to strengthen with infrared spectrum sum of fundamental frequencies area and imitated first on the ITO nano-particles or thin-film material of synthesis
SENIR the and SEIRAS substrates of fruit, its innovative significance is summarized as at 3 points：(1) infrared spectrum in higher energy is interval (whole near
Infrared spectral region) SENIR signals are obtained, the energy match for improving surface enhanced substrate is interval, before not on SENIR's
Report；(2) SEIRAS substrates are extended to semiconductor ITO materials from noble silver, gold, widen base material scope；(3) increase
The strong factor reaches 104, higher than the enhancing ability of the surface enhanced substrate in any infrared spectrum interval being currently known.
Brief description of the drawings
Fig. 1：Acid red probe molecule (10-10Mol/L) SENIR of the modification in ITO nanoparticle powder substrates and
SEIRAS spectrograms (curve a)；Infrared spectrogram (curve b) before acid red is non-reinforced.
Fig. 2：Tonyred probe molecule (10-10Mol/L) SENIR of the modification in ITO nanoparticulate thin films substrates and
SEIRAS spectrograms (curve a)；Infrared spectrogram (curve b) before tonyred is non-reinforced.
Fig. 3：4-Mercaptopyridine probe molecule (10-10Mol/L) SENIR of the modification in ITO nanoparticle powder substrates and
SEIRAS spectrograms (curve a)；Infrared spectrogram (curve b) before 4-Mercaptopyridine is non-reinforced.
Embodiment
With reference to example, the invention will be further elaborated, rather than limits the invention.
Embodiment 1
Infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis, using acid red as the surface of probe molecule
Modify and SENIR and SEIRAS detections are carried out using direct method and pressing potassium bromide troche method.
1st, infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis：
(1) Indium Tris acetylacetonate for taking 0.249g and 0.0261g acetylacetone,2,4-pentanedione stannic chlorides are weighed in the balance.
(2) above-mentioned sample is put into 50mL beaker, and adds 15mL n-Butanol soluble sample, stirred with glass bar
After uniform, ultrasound 10 minutes.
(3) step (2) resulting solution 12mL is measured with graduated cylinder to be fitted into reactor, and reactor is put into constant temperature oven and risen
Temperature continues to heat 48 hours, puts reactor cool down at room temperature afterwards, product is centrifuged, obtain solid product to 200 DEG C.
(4) solid product is then placed in vacuum drying chamber constant temperature 60 by ethanol, alternate three washings of deionized water
DEG C, dry 12 hours, obtain ITO nanoparticle powders 0.094g.
2nd, using acid red as the surface modification of probe molecule：
It is 10 to weigh the ITO nanoparticle powders 0.05g that above-mentioned steps (4) obtain and be added to 10mL concentration-10Mol/L's
In the aqueous solution of acid red probe molecule, magnetic agitation 12 hours is cleaned and centrifuged with deionized water three times, removed and do not inhale
Attached probe molecule, then dries naturally, and obtaining surface modification has the ITO nanoparticle powders of probe molecule.
3rd, SENIR and SEIRAS is carried out using direct method and pressing potassium bromide troche method to detect：
SENIR tests can be directly carried out near infrared region, SEIRAS is carried out using pressing potassium bromide troche method in middle infrared
Test.Tested using pressing potassium bromide troche method, specific tabletting method is：1. first, 200mg KBr and being surveyed for 2mg are taken
Sample, grinds 2 minutes.Note along a direction grinding, in order to avoid destruction crystal structure.Workbench should be equipped with infrared lamp, whole
Completed under infrared lamp baking.2. then, modulus has, wiped clean.Base is installed, interior module smooth surface is put into upwards, medication
Sample is uniformly put into by product spoon, by fore-set plus well, gently can rotate to make sample uniformly spread out.3. mould is placed on tablet press machine
On, spiral is screwed, vent valve is fastened, 20MPa is forced into, stopped 2 minutes.4. it is last, vent valve is slowly opened, makes pressure slow
Drop to 0.Turn on spiral and take out mould.Base is opened, interior module is reversely extruded, the pressure pressed is carefully taken out with the medicine shovel of plane
Piece, is put into tablet folder.
As shown in figure 1, respectively concentration is 10-10Mol/L acid red is modified in ITO nanoparticle powder substrates
(curve a) and concentration are 10 to SENIR and SEIRAS spectrograms-10Infrared spectrum (the curve b) of mol/L acid red body.It can see
Go out, concentration is 10-10Infrared signal is very weak before mol/L acid red is non-reinforced, and enhancing base is used as by the use of ITO nanoparticle powders
Behind bottom, its signal is clearly enhanced.Illustrate that there is new ITO nanoparticle powders substrate higher SENIR and SEIRAS to live
Property, while also demonstrating viewpoint above：We synthesize ITO material free electron densities are big, resistivity is small, with infrared light
Sum of fundamental frequencies area plasmon resonance characteristic is composed, in visible region extinction coefficient very little so that the material is in terms of infrared effect is strengthened
There is good application prospect.
Embodiment 2
Infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis, using tonyred as the surface of probe molecule
Modify and SENIR and SEIRAS detections are carried out using direct method.
1st, infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis：
(1) Indium Tris acetylacetonate for taking 0.249g and 0.0261g acetylacetone,2,4-pentanedione stannic chlorides are weighed in the balance.
(2) above-mentioned sample is put into 50mL beaker, and adds 15mL n-Butanol soluble sample, stirred with glass bar
After uniform, ultrasound 10 minutes.
(3) step (2) resulting solution 12mL is measured with graduated cylinder to be fitted into reactor, and reactor is put into constant temperature oven and risen
Temperature continues to heat 48 hours, puts reactor cool down at room temperature afterwards, product is centrifuged, obtain solid product to 200 DEG C.
(4) solid product is then placed in vacuum drying chamber constant temperature 60 by ethanol, alternate three washings of deionized water
DEG C, dry 12 hours, obtain ITO nanoparticle powders 0.094g.
(5) by obtained ITO nanoparticle powder 188mL deionized water dissolvings, stir 6 hours, obtaining concentration is
0.5g/L ITO nanoparticle sols.
2nd, using tonyred as the surface modification of probe molecule：
The thick silverskin of one layer of 400nm is plated with vacuum coating equipment on the glass sheet first, is dipped the substrate into again after taking-up
20 minutes in 0.01mol/L diallyl dimethyl ammoniumchloride (PDDA) aqueous solution, cleaned after taking-up with deionized water, nitrogen
Air-blowing is done.Then dip the substrate into again in ITO nanoparticle sols 6 hours, cleaned and centrifuged with deionized water after taking-up
Three times, nitrogen drying, obtaining surface self-organization has SENIR the or SEIRAS substrates of ITO nano-particles.Then substrate is dipped into
The 10 of 10mL-10In the ethanol solution of mol/L tonyred, taken out after 8 hours, cleaning three times is carried out with ethanol, is removed unadsorbed
Probe molecule, nitrogen drying, obtaining surface modification has the ITO nanoparticulate thin films of probe molecule.
3rd, SENIR and SEIRAS is carried out using direct method to detect：
SENIR and SEIRAS tests are carried out using direct method.
As shown in Fig. 2 respectively concentration is 10-10Mol/L tonyred is modified in ITO nanoparticulate thin films substrates
(curve a) and concentration are 10 to SENIR and SEIRAS spectrograms-10Infrared spectrum (the curve b) of mol/L tonyred body.From figure
As can be seen that concentration is 10-10Infrared signal is very weak before mol/L tonyred is non-reinforced, and enhancing is used as by the use of ITO nano materials
After substrate, its signal is clearly enhanced.Illustrate that new ITO nanoparticulate thin films substrate has higher SENIR and SEIRAS
Activity.
Embodiment 3
Infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis, using 4-Mercaptopyridine as probe molecule
Surface modification and use direct method and pressing potassium bromide troche method carry out SENIR and SEIRAS detections.
1st, infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis：
Method is with example 1.
2nd, using 4-Mercaptopyridine as the surface modification of probe molecule：
By the 10 of 10 μ L-10The ITO nanoparticle powders in 0.01g are added dropwise in the ethanol solution of mol/L 4-Mercaptopyridine
On, then dry naturally, you can obtaining surface modification there are the ITO nanoparticle powders of probe molecule.
3rd, SENIR and SEIRAS is carried out using direct method and pressing potassium bromide troche method to detect：
SENIR tests can be directly carried out near infrared region, SEIRAS is carried out using pressing potassium bromide troche method in middle infrared
Test.The specific method be the same as Example 1 of tabletting.
As shown in figure 3, respectively concentration is 10-10Mol/L 4-Mercaptopyridine is modified in ITO nano-particle substrates
(curve a) and concentration are 10 to SENIR and SEIRAS spectrograms-10Infrared spectrum (the curve b) of mol/L 4-Mercaptopyridine body.Can
To find out, concentration is 10-10The infrared signal of mol/L 4-Mercaptopyridine body is very weak, and enhancing is used as by the use of ITO nano materials
After substrate, its signal is clearly enhanced.Illustrate that new ITO nano-particles substrate has higher SENIR and SEIRAS activity.
Claims (6)
1. a kind of application ITO nano materials are as the method for infrared spectrum sum of fundamental frequencies area surface enhanced substrate, its step is as follows：
(1) infrared spectrum sum of fundamental frequencies area plasmon resonance nano material ITO synthesis：
(1) 0.1~2.5g Indium Tris acetylacetonate and 0.01~0.27g acetylacetone,2,4-pentanedione stannic chlorides is weighed；
(2) 10~20mL n-butanol, after stirring, ultrasound 10~20 minutes are added into above-mentioned sample；
(3) by step (2) resulting solution at 150~200 DEG C hydro-thermal reaction 30~60 hours, be cooled to after room temperature by product from
The heart, obtains solid product；
(4) solid product by ethanol, deionized water alternately wash, then under 60~80 DEG C of vacuum conditions freeze-day with constant temperature 10~
20 hours, obtain ITO nanoparticle powders；
(5) obtained ITO nanoparticle powders deionized water or organic solvent are dissolved, stirs 4~8 hours, obtain concentration
For 0.1~8.5g/L ITO nanoparticle sols.
(2) surface modification of probe molecule：
Weigh 0.01~0.1g of ITO nanoparticle powders that above-mentioned steps (4) obtain and be added to 10-10~10-2Mol/L probe
In the aqueous solution or ethanol solution of molecule, stir 1~24 hour, be cleaned multiple times with probe molecule solutions identical solvent and from
The heart is separated, and is removed unadsorbed probe molecule, is then dried naturally, obtaining surface modification has the ITO nano-particles of probe molecule
Powder；
Or, 10 that 5~1000 μ L above-mentioned steps (5) are obtained-10~10-2The aqueous solution or ethanol of mol/L probe molecule are molten
Drop is added in 0.01~0.1g ITO nanoparticle powders, is then dried naturally, you can obtaining surface modification has probe molecule
ITO nanoparticle powders；
Or, ITO nano-particles are assembled into substrate by the method for self assembly, substrate is then dipped into 10-10~10- 2In the aqueous solution or ethanol solution of mol/L probe molecule, taken out after 4~12 hours, with molten with probe molecule solutions identical
Agent clean repeatedly, removes unadsorbed probe molecule, and nitrogen is dried up, and obtaining surface modification has the ITO nanometers of probe molecule
Particle film；
Or, it is directly added into 10 in obtained ITO nanoparticle sols-10~10-2The aqueous solution of mol/L probe molecule or
Ethanol solution, is stirred 2~8 hours, you can obtaining surface modification has the ITO nanoparticle sols of probe molecule.
(3) ITO nanoparticle powders, surface modification that surface modification obtained above has probe molecule there is into probe molecule
The ITO nanoparticle sols that ITO nanoparticulate thin films or surface modification have probe molecule increase as infrared spectrum sum of fundamental frequencies area surface
Strong basis bottom carries out SENIR or SEIRAS tests.
2. a kind of application ITO nano materials as claimed in claim 1 are used as the side of infrared spectrum sum of fundamental frequencies area surface enhanced substrate
Method, it is characterised in that：Organic solvent described in step (1) is ethanol, toluene, chloroform or hexamethylene.
3. a kind of application ITO nano materials as claimed in claim 1 are used as the side of infrared spectrum sum of fundamental frequencies area surface enhanced substrate
Method, it is characterised in that：Probe molecule described in step (2) can for mercaptopropionic acid, 6- mercaptohexanoic acids, to mercaptobenzoic acid,
Pyridine, 4-Mercaptopyridine, rhodamine B, rhodamine 6G, acid red or tonyred.
4. a kind of application ITO nano materials as claimed in claim 1 are used as the side of infrared spectrum sum of fundamental frequencies area surface enhanced substrate
Method, it is characterised in that：Self-assembling method described in step (2), is in vacuum condition first on sheet glass or silicon chip substrate
The silver or gold thin film of the μ m-thick of one layer of 10nm of lower evaporation~4, dip the substrate into 0.01~0.1mol/L polydiene third again after taking-up
10~30 minutes in base dimethylammonium chloride aqueous ammonium, cleaned after taking-up with deionized water, nitrogen drying；Then substrate is soaked again
Enter in ITO nanoparticle sols 4~8 hours, cleaned after taking-up with ITO nanoparticle sol identical solvents, nitrogen
Drying, obtaining surface self-organization has the substrate of ITO nano-particles.
5. a kind of application ITO nano materials as claimed in claim 1 are used as the side of infrared spectrum sum of fundamental frequencies area surface enhanced substrate
Method, it is characterised in that：The instrument that SENIR or SEIRAS tests are carried out described in step (3) is Bruker Fourier
Transform Infrared Spectrometer 80v or Bruker Near infrared spectrometer MPA.
6. a kind of application ITO nano materials as claimed in claim 5 are used as the side of infrared spectrum sum of fundamental frequencies area surface enhanced substrate
Method, it is characterised in that：There are the ITO nanoparticle powder samples of probe molecule for surface modification, near infrared region can directly be tested,
Middle infrared is tested using pressing potassium bromide troche method；Surface modification has the ITO nanoparticulate thin films samples of probe molecule, near-infrared
Area and middle infrared can be tested directly；Have the ITO nanoparticle sol samples of probe molecule for surface modification, be by 10~
1000 μ L colloidal sol is dropped on metallic reflection piece, waits it to dry, and near infrared region is directly tested, middle infrared is anti-using infrared sweep angle
Penetrate annex test.
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| Publication number | Priority date | Publication date | Assignee | Title |
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