CN103808968B - For afm tip and the method for making thereof of the metal-modified of Tip-Enhanced Raman Spectroscopy - Google Patents
For afm tip and the method for making thereof of the metal-modified of Tip-Enhanced Raman Spectroscopy Download PDFInfo
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- CN103808968B CN103808968B CN201410054946.6A CN201410054946A CN103808968B CN 103808968 B CN103808968 B CN 103808968B CN 201410054946 A CN201410054946 A CN 201410054946A CN 103808968 B CN103808968 B CN 103808968B
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Abstract
The invention belongs to physical chemistry and near-field raman spectrum field, particularly for the afm tip and preparation method thereof of the metal-modified of Tip-Enhanced Raman Spectroscopy (TERS).The afm tip of metal-modified of the present invention has Cu nanometer film in the finishing of afm tip, has Au or Ag nanometer film in the finishing of Cu nanometer film.The afm tip of the metal-modified for TERS of the present invention, generally can make Raman spectrum strengthen 10 ~ 15 times, is better than only with the afm tip that Au or Ag nanometer film is modified, and this afm tip also can be used for the work such as conduction AFM simultaneously.Preparation method of the present invention has easy, easy manipulation, success ratio high, the Raman spectrum of the afm tip prepared strengthen the property better and stable.
Description
Technical field
The invention belongs to physical chemistry and near-field raman spectrum field, particularly for the afm tip and preparation method thereof of the metal-modified of Tip-Enhanced Raman Spectroscopy (TERS).
Background technology
Atom, molecule are the most elementary cells determining material physicochemical property.At present, scientists, when the physicochemical property of nanoscale molecular level or even single molecules level research material, expects to obtain the key messages such as the pattern of material, chemical composition and chemical constitution simultaneously.But due to restriction and the lower sensitivity of the optical resolution of traditional Raman (Raman) technology, cannot complete material molecule level even In Single-molecular Physics chemically Quality Research at nanoscale; Surface enhanced raman spectroscopy (SERS), cannot at the pattern of Molecular level study material though technology can study the information such as chemical composition, structure of material at nanoscale; Scanning electron microscope (SEM) and transmission electron microscope (TEM), scanning probe microscopy (SPM), though technology can study the pattern of material at nanoscale, cannot obtain the key physical chemical property such as chemical composition, chemical constitution of material simultaneously at nanoscale; Then above-mentioned research can be successfully applied in conjunction with Tip-Enhanced Raman Spectroscopy (TERS) technology of Raman with SPM.When carrying out the research of nanoscale molecular level even single molecules level, TERS technology can obtain the shape appearance figure of material and the Raman spectrogram with a large amount of spectral information simultaneously.
So far, TERS technology obtains widespread use in the various fields such as Surface Science, nanometer technology, bioelectronics, and develops into original position gradually, in real time, studies that material physicochemical property are important, multi-functional technological means under molecular level condition.In the TERS technology studied, TERS(AFM-TERS based on atomic force microscope (AFM)) technology is because of the advantage of AFM technology, the information such as the phasor of material also can be obtained when carrying out TERS research, and this technology is also applicable to atmospheric environment, (surpassing) vacuum/(surpassing) cryogenic conditions, the TERS technology therefore based on AFM is with a wide range of applications and development space.
In AFM-TERS technology, with metal nanoparticle or metal nano film modified after afm tip be the core of this technology.But the modification technique of AFM-TERS needle point still exists some technical barriers to be needed to overcome.At present, the modification of needle point is generally modified Au or the Ag nanometer film with certain roughness by hot evaporation coating method and has been come on needle point, and the TERS that generally can obtain 2 ~ 4 times strengthens the property.But there is unstable, the problem such as plated film easily comes off of evaporation rate of complex operation, metal in hot evaporation coating technique, simultaneously because the material of afm tip mostly is Si or Si
3n
4, the ductility of Au or Ag on needle point and the non-constant of adhesiveness also can cause that Au or Ag excessively assembles, coating easily comes off, the poor repeatability of needle point, prepare the problems such as the success ratio of needle point is low, and these problems directly affects performance or the life-span of needle point.In addition, although there is people to attempt modifying other special material as preparation TERS afm tips such as carbon pipes on needle point, these methods are too loaded down with trivial details, all non-constant of controllability, repeatability, and cost is very high.
The present invention assists the method for modification by metal, can prepare ductility easily and adhesiveness is good, the afm tip of the higher and stable metal-modified for TERS of strengthening the property.
Summary of the invention
An object of the present invention is to provide the afm tip that the metal (Au or Ag and Cu) for Tip-Enhanced Raman Spectroscopy (TERS) is modified.
Two of object of the present invention is to provide with magnetron sputtering method and using Cu as substrate, the method for the afm tip that the metal (Au or Ag and Cu) for the preparation of Tip-Enhanced Raman Spectroscopy (TERS) is modified.
The afm tip of the metal-modified for Tip-Enhanced Raman Spectroscopy (TERS) of the present invention has Cu nanometer film in the finishing of afm tip, has Au or Ag nanometer film in the finishing of Cu nanometer film.
The thickness of described Cu nanometer film is preferably 1 ~ 10nm.
The thickness of described Au or Ag nanometer film is preferably 10 ~ 50nm.
The preparation method of the afm tip of the metal-modified for Tip-Enhanced Raman Spectroscopy (TERS) of the present invention:
Afm tip is fixed in the sample panel in magnetic control sputtering device, Cu and Au or Ag target are placed in 2 target chambeies respectively, first on afm tip, Slag coating obtains Cu nanometer film, the condition of work of magnetic control sputtering device is: under inert gas (as Ar) protection, working pressure is 0.1 ~ 1Pa, and DC electric power is 50 ~ 100W; Then on the afm tip that finishing has Cu nanometer film, Slag coating obtains Au or Ag nanometer film immediately, and the condition of work of magnetic control sputtering device is: under inert gas (as Ar) protection, working pressure is 0.01 ~ 0.8Pa, and DC electric power is 50 ~ 100W.
Distance between described afm tip and Cu and Au or Ag target is all preferably 100 ~ 500mm.
The sputter temperature of described magnetic control sputtering device when preparing Cu nanometer film and preparation Au or Ag nanometer film is preferably 30 ~ 300 DEG C.
Described sputtering time when preparing Cu nanometer film is preferably 10 ~ 100s.
Described sputtering time when preparing Au or Ag nanometer film is preferably 100 ~ 550s.
The pressure of the master-control room in described magnetic control sputtering device is preferably 1 × 10
-7~ 1 × 10
-3pa.
Described afm tip, before being fixed in magnetic control sputtering device, first can carry out purified treatment.
Described purified treatment is positioned in plasma by afm tip, and with argon plasma air-flow purified treatment afm tip, its purification condition is: radio-frequency power is 25 ~ 75W, pressure is 0.1 ~ 3.5Pa, the time of purified treatment is 5 ~ 50min; Or afm tip is positioned in UV ozone machine, with the pollutant on ultraviolet light and ozone decomposed and oxidation afm tip, its condition of work is: UV power is 100 ~ 150W, the flow of oxygen is 100 ~ 600ml/min, temperature is 20 ~ 100 DEG C, the time of purified treatment is 10 ~ 60min.
The afm tip of the metal-modified for TERS of the present invention, substrate when being using Cu nanometer film as sputtering Au or Ag nanometer film, Raman spectrum generally can be made to strengthen 10 ~ 15 times, and its Raman spectrum that generally only can obtain 2 ~ 4 times of afm tip only modified with Au or Ag nanometer film strengthens result, therefore, the afm tip that Au or Ag nanometer film and Cu nanometer film are modified is better than the afm tip that Au or Ag nanometer film is modified in the performance of TERS, and this afm tip also can be used for the work such as conduction AFM simultaneously; The success ratio of the method for this afm tip modification is simultaneously high, can up to 70%.Preparation method of the present invention has easy, easy manipulation, success ratio high, the Raman spectrum of the afm tip prepared strengthen the property better and stable.
Accompanying drawing explanation
Fig. 1. the Graphene of the afm tip after the Au-Cu modification of the embodiment of the present invention 1 strengthens Raman spectrum.
Fig. 2. the Graphene of the afm tip after the Au modification of comparative example 1 strengthens Raman spectrum.
Fig. 3. the SEM figure of the afm tip after the Ag-Cu modification of the embodiment of the present invention 2.
Fig. 4. the Graphene of the afm tip after the Ag-Cu modification of the embodiment of the present invention 2 strengthens Raman spectrum.
Fig. 5. the Graphene of the afm tip of the Ag modification of comparative example 2 strengthens Raman spectrum.
Fig. 6. the Graphene of the afm tip after the Au-Cu modification of the embodiment of the present invention 3 strengthens Raman spectrum.
Fig. 7. the Graphene of the afm tip after the Au modification of comparative example 3 strengthens Raman spectrum.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described material, all can obtain from commercial channels, adopts commercial afm tip (purchased from Nanosensor company of Switzerland) in experiment.
Embodiment 1
(1) clean:
Be positioned over by afm tip in UV ozone machine, with the pollutant on ultraviolet light and ozone decomposed and oxidation afm tip, its condition of work is: UV power is 110W, the flow of oxygen is 200ml/min, temperature is 50 DEG C, the time of purified treatment is 20min.
(2) decorated nanometer metal film
Afm tip after cleaning is fixed in the sample panel in magnetic control sputtering device, Cu and Au target is placed in respectively 2 target chambeies of magnetic control sputtering device, distance between afm tip and Cu and Au target is 300mm, and the pressure of the master-control room in magnetic control sputtering device is 1 × 10
-6pa; First on afm tip, Slag coating obtains Cu nanometer film, and the condition of work of magnetic control sputtering device is: under argon shield, and working pressure is 0.5Pa, and DC electric power is 100W, and sputter temperature is 40 DEG C, and sputtering time is 20s; Then on the afm tip that finishing has Cu nanometer film, Slag coating obtains Au nanometer film immediately, and the condition of work of magnetic control sputtering device is: under argon shield, and working pressure is 1Pa, and DC electric power is 60W, and sputter temperature is 40 DEG C, and sputtering time is 550s; Finally obtain having thickness to be the Cu nanometer film of 10nm in the finishing of afm tip, have thickness to be the afm tip that the Au-Cu for TERS of the Au nanometer film of 50nm modifies in the finishing of Cu nanometer film.
Take Graphene as sample, expose 0.5s, study strengthening the property of the Raman spectrum of the afm tip that this Au-Cu modifies under the power wavelength that is 2mw is the laser of 532nm, what the Graphene of the afm tip that this Au-Cu modifies strengthened Raman spectrum the results are shown in Figure 1.
Comparative example 1
Substantially identical with embodiment 1, the surface being afm tip after cleaning is not modified with the Cu nanometer film that thickness is 10nm, and what obtain is only be modified with the afm tip that thickness is the Au modification of the Au nanometer film of 50nm on the surface of afm tip.
Study the method for strengthening the property of Raman spectrum of the afm tip that this Au modifies with embodiment 1, what the Graphene of the afm tip that this Au modifies strengthened Raman spectrum the results are shown in Figure 2.
Embodiment 2
(1) clean:
Be positioned over by afm tip in plasma, with Ar plasma flow purified treatment afm tip, its purification condition is: under be 40W and pressure being the condition of 1.2Pa at radio-frequency power, purified treatment 20 minutes.
(2) modified metal nanometer film
Afm tip after cleaning is fixed in the sample panel in magnetic control sputtering device, Cu and Ag target is placed in respectively 2 target chambeies of magnetic control sputtering device, distance between afm tip and Cu and Ag target is 300mm, and the pressure of the master-control room in magnetic control sputtering device is 5 × 10
-6pa; First on afm tip, Slag coating obtains Cu nanometer film, and the condition of work of magnetic control sputtering device is: under argon shield, and working pressure is 0.5Pa, and DC electric power is 60W, and sputter temperature is 40 DEG C, and sputtering time is 10s; Then on the afm tip that finishing has Cu nanometer film, Slag coating obtains Ag nanometer film immediately, and the condition of work of magnetic control sputtering device is: under argon shield, and working pressure is 1Pa, and DC electric power is 75W, and sputter temperature is 40 DEG C, and sputtering time is 100s; Finally obtain having thickness to be the Cu nanometer film of 1nm in the finishing of afm tip, have thickness to be the afm tip that the Ag-Cu for TERS of the Ag nanometer film of 10nm modifies in the finishing of Cu nanometer film, the SEM figure of the afm tip after this Ag-Cu modifies is shown in Fig. 3.
Take Graphene as sample, expose 0.5s, study strengthening the property of the Raman spectrum of the afm tip that this Ag-Cu modifies under the power wavelength that is 2mw is the laser of 532nm, what the Graphene of the afm tip that this Ag-Cu modifies strengthened Raman spectrum the results are shown in Figure 4.
Comparative example 2
Substantially identical with embodiment 2, the surface being afm tip after cleaning is not modified with the Cu nanometer film that thickness is 1nm, and what obtain is only be modified with the afm tip that thickness is the Ag modification of the Ag nanometer film of 10nm on the surface of afm tip.
Study the method for strengthening the property of Raman spectrum of the afm tip that this Ag modifies with embodiment 2, what the Graphene of the afm tip that this Ag modifies strengthened Raman spectrum the results are shown in Figure 5.
Embodiment 3
Substantially identical with embodiment 1, the condition just when decorated nanometer metal film is distinguished as:
During Slag coating Cu nanometer film, DC electric power changes 75w into by 100W, and sputtering time changes 40s into by 20s; During Slag coating Au nanometer film, sputtering time changes 220s into by 550s.
Finally obtain having thickness to be the Cu nanometer film of 5nm in the finishing of afm tip, have thickness to be the afm tip that the Au-Cu for TERS of the Au nanometer film of 20nm modifies in the finishing of Cu nanometer film.
Study method that the Raman spectrum of afm tip that this Au-Cu modifies strengthens the property with embodiment 1, what the Graphene of the afm tip that this Au-Cu modifies strengthened Raman spectrum the results are shown in Figure 6.
Comparative example 3
Substantially identical with embodiment 3, the surface being afm tip after cleaning is not modified with the Cu nanometer film that thickness is 5nm, and what obtain is only be modified with the Au nanometer film that thickness is 20nm on the surface of afm tip.
Study method that the Raman spectrum of afm tip that this Au modifies strengthens the property with embodiment 3, what the Graphene of the afm tip that this Au modifies strengthened Raman spectrum the results are shown in Figure 7.
Foregoing is only the preferred embodiments of the present invention; not for limiting embodiment of the present invention; those of ordinary skill in the art is according to central scope of the present invention and spirit; can carry out corresponding flexible or amendment very easily, therefore protection scope of the present invention should be as the criterion with the protection domain required by claims.
Claims (10)
1. for an afm tip for the metal-modified of Tip-Enhanced Raman Spectroscopy, it is characterized in that: with Si or Si
3n
4finishing for the afm tip of material has Cu nanometer film, has Au or Ag nanometer film in the finishing of Cu nanometer film.
2. the afm tip of the metal-modified for Tip-Enhanced Raman Spectroscopy according to claim 1, is characterized in that: the thickness of described Cu nanometer film is 1 ~ 10nm.
3. the afm tip of the metal-modified for Tip-Enhanced Raman Spectroscopy according to claim 1, is characterized in that: the thickness of described Au or Ag nanometer film is 10 ~ 50nm.
4. the preparation method of the afm tip of the metal-modified for Tip-Enhanced Raman Spectroscopy described in a claims 1 to 3 any one, it is characterized in that: afm tip is fixed in the sample panel in magnetic control sputtering device, Cu and Au or Ag target are placed in 2 target chambeies respectively; First on afm tip, Slag coating obtains Cu nanometer film, and the condition of work of magnetic control sputtering device is: under inert gas shielding, and working pressure is 0.1 ~ 1Pa, and DC electric power is 50 ~ 100W; Then have Slag coating on the afm tip of Cu nanometer film to obtain Au or Ag nanometer film in finishing, the condition of work of magnetic control sputtering device is: under inert gas shielding, and working pressure is 0.01 ~ 0.8Pa, and DC electric power is 50 ~ 100W.
5. preparation method according to claim 4, is characterized in that: the distance between described afm tip and Cu and Au or Ag target is all 100 ~ 500mm.
6. preparation method according to claim 4, is characterized in that: the sputter temperature of described magnetic control sputtering device when preparing Cu nanometer film and preparation Au or Ag nanometer film is 30 ~ 300 DEG C.
7. the preparation method according to claim 4 or 6, is characterized in that: sputtering time during described preparation Cu nanometer film is 10 ~ 100s.
8. the preparation method according to claim 4 or 6, is characterized in that: sputtering time when described preparation Au or Ag nanometer film is 100 ~ 550s.
9. preparation method according to claim 4, is characterized in that: the pressure of the master-control room in described magnetic control sputtering device is 1 × 10
-7~ 1 × 10
-3pa.
10. preparation method according to claim 4, is characterized in that: described afm tip, before being fixed in magnetic control sputtering device, first carries out purified treatment;
Described purified treatment is positioned in plasma by afm tip, and with argon plasma air-flow purified treatment afm tip, its purification condition is: radio-frequency power is 25 ~ 75W, pressure is 0.1 ~ 3.5Pa, the time of purified treatment is 5 ~ 50min; Or afm tip is positioned in UV ozone machine, with the pollutant on ultraviolet light and ozone decomposed and oxidation afm tip, its condition of work is: UV power is 100 ~ 150W, the flow of oxygen is 100 ~ 600ml/min, temperature is 20 ~ 100 DEG C, the time of purified treatment is 10 ~ 60min.
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| CN106645809A (en) * | 2016-10-14 | 2017-05-10 | 厦门大学 | Preparation method for isolated needle point with housing layers wrapped in dual manner |
| CN108375687B (en) * | 2018-03-09 | 2020-12-04 | 北京协同创新研究院 | Method for coating graphene on probe tip of atomic force microscope |
| CN109112491B (en) * | 2018-07-19 | 2019-10-11 | 西安交通大学 | Overstable silver-colored tantalum composite material surface enhancing Raman scattering substrate and preparation method |
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