CN114199854A - Preparation method of SERS substrate constructed by flexible transparent cone ordered array - Google Patents
Preparation method of SERS substrate constructed by flexible transparent cone ordered array Download PDFInfo
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- CN114199854A CN114199854A CN202111539434.5A CN202111539434A CN114199854A CN 114199854 A CN114199854 A CN 114199854A CN 202111539434 A CN202111539434 A CN 202111539434A CN 114199854 A CN114199854 A CN 114199854A
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- 239000000758 substrate Substances 0.000 title claims abstract description 36
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000001020 plasma etching Methods 0.000 claims abstract description 21
- 150000002500 ions Chemical class 0.000 claims abstract description 14
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000012546 transfer Methods 0.000 claims abstract description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 229910052737 gold Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000002474 experimental method Methods 0.000 claims description 8
- 239000002086 nanomaterial Substances 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 238000001237 Raman spectrum Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 3
- 239000004793 Polystyrene Substances 0.000 abstract 5
- 229920002223 polystyrene Polymers 0.000 abstract 1
- 229910018503 SF6 Inorganic materials 0.000 description 29
- 238000007747 plating Methods 0.000 description 25
- 239000010931 gold Substances 0.000 description 19
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 16
- 229960000909 sulfur hexafluoride Drugs 0.000 description 15
- 238000005530 etching Methods 0.000 description 11
- 239000000523 sample Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 6
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 239000000447 pesticide residue Substances 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000012055 fruits and vegetables Nutrition 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Images
Classifications
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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
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention provides a preparation method of an SERS substrate constructed by a flexible transparent cone ordered array, which comprises the following steps of 1, firstly carrying out ultrasonic cleaning on a cut PI film, preparing PS ball liquid with the specification of 500nm, and keeping the PI film for later use after the PI film is cleaned and dried. And 2, carrying out PS (polystyrene) ball transfer on the cleaned PI film, and paving the PS balls on the surface of the PI film for later use. Step 3, carrying out reactive ion etching on the PI film with the spread PS balls, wherein the used gas is SF6And O2Wherein, SF6Flow rate of 40sccm, O2The flow rate was 20 sccm. And 4, carrying out magnetron sputtering coating on the PI film etched by the reactive ions. The substrate meets the flexible and transparent condition, PI (polyimide film) is used as a main material, and the surface of the substrate is in an ordered structure array with hollow cones.
Description
Technical Field
The invention designs a preparation method of an SERS substrate constructed by a flexible transparent cone ordered array. Rather, the SERS substrate formed by experimental conditions were changed in a reactive ion etcher by spreading PS spheres on a PI (polyimide film) film.
Background
Surface Enhanced Raman Scattering (SERS) is an effective, ultrasensitive, label-free fingerprint spectroscopy technique, has been proven to be an attractive chemical and biological analysis tool at present, and has broad application prospects in the fields of biomedicine, material science, surface science, environmental monitoring, explosives, and the like.
The SERS technology overcomes the problem of low sensitivity of common Raman spectrum, thereby greatly enhancing the intensity of original Raman signal and opening up a new path in the analysis and research in the fields of environmental science, life science, safety monitoring and the like.
Due to the advantages of high sensitivity and rapid detection, SERS is expected to be applied to solving the problems of in-situ and trace detection of pesticide residue molecules.
Using SERS detection techniques, the problems of SERS substrates must be circumvented. The pesticide residue molecules are attached to the surfaces of fruits and vegetables, the curvatures and the shapes of different food surfaces are different, and the traditional rigid SERS substrate cannot fully contact the surfaces of the fruits and vegetables with metal, so that the pesticide residue molecules cannot be positioned in an enhanced region of the metal surface; in addition, if in-situ detection is realized, laser needs to be injected from the back surface of the substrate, and the two requirements are that the SERS substrate needs to satisfy the condition of flexible transparency.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for manufacturing a SERS substrate, wherein the substrate meets the flexible and transparent condition, a PI (polyimide film) is used as a main material, and the surface of the substrate is in an ordered structure array with a hollow cone.
The invention adopts the following technical scheme:
a preparation method of an SERS substrate constructed by a flexible transparent cone ordered array comprises the following steps:
step 1, firstly, carrying out ultrasonic cleaning on a cut PI film (polyimide film), preparing PS ball liquid with the specification of 500nm, and reserving after the film is cleaned and dried;
step 2, carrying out PS ball transfer on the cleaned PI, and paving the PS balls on the surface of the PI for later use;
step 3, carrying out reactive ion etching on the PI paved with the PS balls, wherein the used gas is SF6(Sulfur hexafluoride) and O2(oxygen), wherein, SF6Flow rate of 40sccm, O2The flow rate is 20 sccm;
step 4, the power used for reactive ion etching is 150W;
step 5, performing magnetron sputtering coating on the etched PI;
step 6, observing the PI after the experiment under a scanning electron microscope to obtain a nano-structure image;
step 7, immersing the sample etched for 180s in 10-6Raman spectra of different positions in the mol/l ATP solution.
Furthermore, the SERS substrate prepared by the method is a flexible transparent substrate formed by an ordered array of hollow cones.
Further, the thickness of the PI film in step 1 was 20 μm.
Further, the metals deposited in the magnetron sputtering coating in the step 5 are Au and Ag, and the deposition time is respectively 50s and 100 s.
Further, 500nm PS spheres were used in step 1, and were formed by changing experimental conditions in reactive ion etching.
The invention has the beneficial effects that:
the invention provides a method for preparing a 3D flexible transparent SERS substrate on a PI flexible transparent substrate by using a single-layer colloid crystal template as a mask and adopting a strategy of combining reactive ion etching and sputtering deposition. By utilizing the method, the constructed substrate can realize the stability, consistency and high activity of the substrate, has the characteristics of flexibility and transparency, is easy to be attached to the surfaces of vegetables and fruits, meets the condition of adsorbing pesticide residue molecules on the surface of noble metal, and realizes the in-situ trace detection of the pesticide residue molecules.
Drawings
FIG. 1 is a field emission scanning electron micrograph of a typical flexible transparent SERS substrate prepared;
FIG. 2 is a field emission scanning electron micrograph of a sample prepared under other conditions;
FIG. 3 is a field emission scanning electron micrograph of a sample prepared under other conditions;
FIG. 4 is a field emission scanning electron micrograph of a sample prepared under other conditions;
FIG. 5 is a field emission scanning electron micrograph of a sample prepared under other conditions;
FIG. 6 is a field emission scanning electron micrograph of a sample prepared under other conditions;
FIG. 7 shows the flexible transparent SERS substrate of FIG. 1 at 10-6(mol/l) Raman spectra of different positions in the ATP solution;
FIG. 8 is a flow chart of the steps of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described below clearly and completely, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 8, examples 1 to 6 describe in detail the process flow of SERS substrate constructed by flexible transparent cone ordered array, experimental articles and equipments: PI (polyimide film), reactive ion etcher, plasma magnetron sputtering coating instrument, ultrasonic cleaner, ultrapure water machine and SF (sulfur hexafluoride)6Gas, O2。
Example 1
The experimental steps are as follows:
(1) firstly, carrying out ultrasonic cleaning on a cut PI (polyimide film) film, preparing PS ball liquid with the specification of 500nm, and then, after the film is cleaned and dried, keeping the film for later use.
(2) And (4) carrying out PS ball transfer on the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Putting the PI with the PS balls inPerforming reactive ion etching with sulfur hexafluoride (SF) as gas6) And oxygen (O)2) Wherein, SF6Flow rate of 40sccm, O2The flow rate was 20 sccm.
(4) The power used for reactive ion etching was 150W.
(5) Performing magnetron sputtering plating (Au, Ag) film on the etched PI, and finally selecting after multiple tests; au plating for 50 seconds, then Ag plating for 100 seconds.
(6) The PI after the experiment was observed under a scanning electron microscope to obtain a nanostructure image, as shown in fig. 1.
In FIG. 1, 500nm PS spheres are used as mask, SF6Flow rate of 40sccm, O2The flow rate is 20sccm, the power of the reactive ion etcher is 150W, the etching time is 180 seconds respectively, and the film plating is to plate Au for 50 seconds and then plate Ag for 100 seconds;
(7) the sample etched for 180 seconds was immersed in 10-6(mol/l) Raman spectra of different positions in 4-ATP solution, as shown in FIG. 7.
Example 2
The experimental steps are as follows:
(1) firstly, performing ultrasonic cleaning on a cut PI (polyimide film) film, preparing PS ball liquid with the specification of 500nm, and then, after the film is cleaned and dried, reserving the film for later use.
(2) And (4) carrying out PS ball transfer on the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI with spread PS balls, wherein the used gas is sulfur hexafluoride (SF)6) And oxygen (O)2) Wherein, SF6Flux of 40sccm, O2The flux is 20ccm, the power of the reactive ion etcher is 150W, and the etching time is 120 seconds respectively.
(4) The power used for reactive ion etching was 150W.
(5) And (3) carrying out magnetron sputtering plating (Au, Ag) on the etched PI for 50 seconds, and then plating Ag for 100 seconds.
(6) The PI after the experiment was observed under a scanning electron microscope to obtain a nanostructure image, as shown in fig. 2.
In fig. 2, the preparation conditions are: at 500nm PS spheres as mask, SF6Flow rate of 40sccm, O2The flow rate is 20sccm, the power of the reactive ion etcher is 150W, the etching time is 120 seconds respectively, and the plating is to plate Au for 50 seconds and then plate Ag for 100 seconds;
example 3
The experimental steps are as follows:
(1) firstly, performing ultrasonic cleaning on a cut PI (polyimide film) film, preparing PS ball liquid with the specification of 500nm, and then, after the film is cleaned and dried, reserving the film for later use.
(2) And (4) carrying out PS ball transfer on the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI with spread PS balls, wherein the used gas is sulfur hexafluoride (SF)6) And oxygen (O)2) Wherein, SF6Flux of 40sccm, O2The flux is 20ccm, the power of the reactive ion etcher is 150W, and the etching time is 60 seconds respectively.
(4) The power used for reactive ion etching was 150W.
(5) And (3) carrying out magnetron sputtering plating (Au, Ag) on the etched PI for 50 seconds, and then plating Ag for 100 seconds.
(6) The PI after the experiment was observed under a scanning electron microscope to obtain a nanostructure image, as shown in fig. 3.
In fig. 3, the preparation conditions are: using 500nm PS spheres as mask, SF6Flow rate of 40sccm, O2The flow rate is 20sccm, the power of the reactive ion etcher is 150W, the etching time is 60 seconds respectively, and the plating is to plate Au for 50 seconds and then plate Ag for 100 seconds.
Example 4
The experimental steps are as follows:
(1) firstly, performing ultrasonic cleaning on a cut PI (polyimide film) film, preparing PS ball liquid with the specification of 500nm, and then, after the film is cleaned and dried, reserving the film for later use.
(2) And (4) carrying out PS ball transfer on the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI with spread PS balls, wherein the used gas is sulfur hexafluoride (SF)6) And oxygen (O)2) Wherein, SF6Flux 60sccm, O2The flux was 20sccm, the reactive ion etcher power was 180W, and the etching time was 180 seconds, respectively.
(4) The power used for reactive ion etching was 180W.
(5) And (3) carrying out magnetron sputtering plating (Au, Ag) on the etched PI for 50 seconds, and then plating Ag for 100 seconds.
(6) The PI after the experiment was observed under a scanning electron microscope to obtain a nanostructure image, as shown in fig. 4.
In fig. 4, the preparation conditions are: SF6The flow rate was 60sccm, O2The flow rate is 20sccm, the power of the reactive ion etching machine is 180W, and the etching time is 180 seconds respectively; the plating is performed by first plating Au for 50 seconds and then plating Ag for 100 seconds.
Example 5
The experimental steps are as follows:
(1) firstly, performing ultrasonic cleaning on a cut PI (polyimide film) film, preparing PS ball liquid with the specification of 500nm, and then, after the film is cleaned and dried, reserving the film for later use.
(2) And (4) carrying out PS ball transfer on the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI with spread PS balls, wherein the used gas is sulfur hexafluoride (SF)6) And oxygen (O)2) Wherein, SF6Flux 60sccm, O2The flux was 20sccm, the reactive ion etcher power was 180W, and the etching time was 120 seconds, respectively.
(4) The power used for reactive ion etching was 180W.
(5) And (3) carrying out magnetron sputtering plating (Au, Ag) on the etched PI for 50 seconds, and then plating Ag for 100 seconds.
(6) The PI after the experiment was observed under a scanning electron microscope to obtain a nanostructure image, as shown in fig. 5.
In fig. 5, the preparation conditions are: SF6The flow rate was 60sccm, O2The flow rate is 20sccm, the power of the reactive ion etcher is 180W, and the etching time is 120 seconds respectively; the plating is performed by first plating Au for 50 seconds and then plating Ag for 100 seconds.
Example 6
The experimental steps are as follows:
(1) firstly, performing ultrasonic cleaning on a cut PI (polyimide film) film, preparing PS ball liquid with the specification of 500nm, and then, after the film is cleaned and dried, reserving the film for later use.
(2) And (4) carrying out PS ball transfer on the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI with spread PS balls, wherein the used gas is sulfur hexafluoride (SF)6) And oxygen (O)2) Wherein, SF6Flux 60sccm, O2The flux is 20ccm, the power of the reactive ion etcher is 180W, and the etching time is 60 seconds respectively.
(4) The power used for reactive ion etching was 180W.
(5) And (3) carrying out magnetron sputtering plating (Au, Ag) on the etched PI for 50 seconds, and then plating Ag for 100 seconds.
(6) The PI after the experiment was observed under a scanning electron microscope to obtain a nanostructure image, as shown in fig. 6.
In FIG. 6, SF6The flow rate was 60sccm, O2The flow rate is 20sccm, the power of the reactive ion etcher is 180W, and the etching time is 60 seconds respectively; the plating is performed by first plating Au for 50 seconds and then plating Ag for 100 seconds.
In summary, in fig. 1, the period of the ordered array structure constructed by the cones is 500nm, and the surface is rough gold and silver nanoparticles. As can be seen from the two broken photographs in the figure, the cone is a hollow structure.
In fig. 2, the period of the ordered array structure constructed by the quasi-cylinders is 500nm, and the surface of the ordered array structure is rough gold and silver nano-particles. The cylinder is of solid construction.
In fig. 3, the ordered array structure constructed by the cone has a period of 500nm and a rough surface of gold and silver nanoparticles. The cone is of solid construction and the size of the cone is reduced relative to figure 1.
In fig. 4, the period of the ordered array structure constructed by the broken cylinder is 500nm, and the surface is rough gold and silver nanoparticles. With respect to fig. 2, the array is constructed of a broken hollow cylinder structure.
In fig. 5, the period of the ordered array structure constructed by the broken cone is 500nm, and the surface of the ordered array structure is rough gold and silver nano-particles. With respect to fig. 1, the array is constructed as a broken hollow cone structure.
In FIG. 6, the ordered array structure constructed by the cone has a period of 500nm and a rough surface of gold and silver nanoparticles. With respect to fig. 1 and 3, the cone is a solid structure and the surface is composed of nanowires.
FIG. 7 is a Raman spectrum obtained with the substrate of FIG. 1 and 4-ATP as the probe molecule. In addition, the Raman spectrum of 4-ATP was not obtained under the same conditions using other substrates. In conclusion, only in the case of example 1, a flexible transparent cone ordered array structure can be obtained, and the structure has better SERS performance.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of an SERS substrate constructed by a flexible transparent cone ordered array is characterized by comprising the following steps:
step 1, firstly, carrying out ultrasonic cleaning on the cut PI film, preparing PS ball liquid with the specification of 500nm, and keeping the PI film for later use after the PI film is cleaned and dried;
step 2, carrying out PS ball transfer on the cleaned PI film, and paving the PS balls on the surface of the PI film for later use;
step 3, carrying out reactive ion etching on the PI film with the spread PS balls, wherein the used gas is SF6And O2Wherein, SF6Flow rate of 40sccm, O2The flow rate is 20 sccm;
and 4, carrying out magnetron sputtering coating on the PI film etched by the reactive ions.
2. The method for preparing a SERS substrate constructed by the flexible and transparent cone ordered array according to claim 1, wherein in the step 1, the thickness of the PI film is 20 μm.
3. The method for preparing a SERS substrate constructed by the flexible transparent cone ordered array according to claim 1, wherein the PS spheres with the specification of 500nm used in the step 1 are used as masks and are formed by changing experimental conditions in reactive ion etching.
4. The method for preparing a SERS substrate constructed by the flexible and transparent cone ordered array according to claim 1, wherein in the step 3, the power used for reactive ion etching is 150W.
5. The method for preparing a SERS substrate constructed by the ordered array of flexible transparent cones according to claim 1, wherein in the step 5, the metals deposited in the magnetron sputtering coating are Au and Ag, and the deposition time is 50s and 100s respectively.
6. The method for preparing the SERS substrate constructed by the flexible and transparent cone ordered array according to claim 1, further comprising observing the PI film after the experiment under a scanning electron microscope to obtain a nano-structure image.
7. The method for preparing a SERS substrate constructed by the flexible and transparent cone ordered array according to claim 1, further comprising immersing a sample etched for 180s in 10-6Raman spectra of different positions in the mol/l ATP solution.
8. The method for preparing the SERS substrate constructed by the flexible and transparent conical ordered array according to any one of claims 1 to 7, wherein the prepared SERS substrate is a flexible and transparent substrate with the hollow conical ordered array.
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