CN114199854B - 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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- CN114199854B CN114199854B CN202111539434.5A CN202111539434A CN114199854B CN 114199854 B CN114199854 B CN 114199854B CN 202111539434 A CN202111539434 A CN 202111539434A CN 114199854 B CN114199854 B CN 114199854B
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- 239000000758 substrate Substances 0.000 title claims abstract description 31
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001020 plasma etching Methods 0.000 claims abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 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 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000012546 transfer Methods 0.000 claims abstract description 3
- 238000005530 etching Methods 0.000 claims description 12
- 239000002086 nanomaterial Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 3
- 239000010931 gold Substances 0.000 description 20
- 238000007747 plating Methods 0.000 description 12
- 230000004907 flux Effects 0.000 description 10
- 229910018503 SF6 Inorganic materials 0.000 description 9
- 229910052737 gold Inorganic materials 0.000 description 9
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 9
- 229960000909 sulfur hexafluoride Drugs 0.000 description 9
- 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
- 238000001237 Raman spectrum Methods 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000000447 pesticide residue Substances 0.000 description 5
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000012055 fruits and vegetables 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
- 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
- 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
Classifications
-
- 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 a SERS substrate constructed by a flexible transparent cone ordered array, which comprises the following steps of 1, firstly, carrying out ultrasonic cleaning on a sheared PI film, simultaneously preparing PS sphere liquid with the specification of 500nm, and after the PI film is cleaned and dried, keeping the PI film for later use. And step 2, performing PS ball transfer on the cleaned PI film, and paving PS balls on the surface of the PI film for later use. Step 3, performing reactive ion etching on the PI film paved with the PS balls, wherein the gas is SF 6 And O 2 Wherein SF is 6 Flow rate is 40sccm, O 2 The flow rate was 20sccm. And 4, performing magnetron sputtering coating on the PI film etched by the reactive ions. The substrate meets the condition of flexibility and transparency, takes PI (polyimide film) as a main material, and has an ordered structure array with hollow cones on the surface.
Description
Technical Field
The invention designs a preparation method of a SERS substrate constructed by a flexible transparent cone ordered array. Rather, the SERS substrate formed by changing experimental conditions in a reactive ion etcher by laying PS spheres on PI (polyimide film) film.
Background
Surface Enhanced Raman Scattering (SERS) is an effective, ultrasensitive, label-free fingerprint spectroscopy technique, which has been proven to be an attractive chemical and biological analysis tool at present, and has a wide application prospect 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 the common Raman spectrum, so that the intensity of the original Raman signal can be greatly enhanced, and a new path is opened up in 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 solve the problems of in-situ and trace detection of pesticide residue molecules.
The problem of SERS substrates must not be bypassed using SERS detection techniques. Because pesticide residue molecules are attached to the surfaces of fruits and vegetables, the curvatures and the shapes of the surfaces of different foods are different, and the traditional rigid SERS substrate cannot be fully contacted with the surfaces of the fruits and the vegetables, so that the enhancement region of the pesticide residue molecules on the surfaces of the metals cannot be realized; in addition, if in situ detection is achieved, laser light is required to be incident from the back of the substrate, both of which require that the SERS substrate must meet the conditions of flexibility and transparency.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provide a manufacturing method of a SERS substrate, wherein the substrate meets the condition of flexibility and transparency, PI (polyimide film) is used as a main material, and the surface of the substrate is an ordered structure array with hollow cones.
The invention adopts the following technical scheme:
a preparation method of a SERS substrate constructed by a flexible transparent cone ordered array comprises the following steps:
step 1, firstly, performing ultrasonic cleaning on a sheared PI film (polyimide film), preparing PS sphere liquid with the specification of 500nm, and after the film is cleaned and dried, keeping the film for later use;
step 2, PS ball transfer is carried out on the cleaned PI, and PS balls are paved on the surface of the PI for standby;
step 3, performing reactive ion etching on PI paved with PS balls, wherein the gas is SF 6 (Sulfur hexafluoride) and O 2 (oxygen), wherein SF 6 Flow rate is 40sccm, O 2 The flow rate is 20sccm;
step 4, the power used by the reactive ion etching is 150W;
step 5, performing magnetron sputtering coating on the etched PI;
step 6, observing the experimental PI under a scanning electron microscope to obtain a nanostructure image;
step 7, immersing the sample etched for 180s in the solution 10 -6 Raman spectra at different positions in the mol/l ATP solution.
Furthermore, the SERS substrate prepared by the method is a flexible transparent substrate which is provided with a hollow cone ordered array.
Further, the thickness of the PI film in step 1 was 20. Mu.m.
Further, metals deposited in the magnetron sputtering coating in the step 5 are Au and Ag, and the deposition time is 50s and 100s respectively.
Further, the PS spheres of 500nm used in step 1 were formed by changing experimental conditions in reactive ion etching.
The invention has the beneficial effects that:
the invention provides a preparation method of a 3D flexible transparent SERS substrate by taking a single-layer colloidal crystal template as a mask on a PI flexible transparent substrate and combining reactive ion etching and sputter deposition. The substrate constructed by the method not only can realize the stability, consistency and high activity of the substrate, but also has the characteristics of flexibility and transparency, is easy to be attached to the surfaces of vegetables and fruits, meets the condition that pesticide residue molecules are adsorbed on the surfaces of noble metals, and realizes the in-situ trace detection of the pesticide residue molecules.
Drawings
FIG. 1 is a field emission scanning electron microscope image of a typical flexible transparent SERS substrate prepared;
FIG. 2 is a field emission scanning electron microscope image of a sample prepared under other conditions;
FIG. 3 is a field emission scanning electron microscope image of a sample prepared under other conditions;
FIG. 4 is a field emission scanning electron microscope image of a sample prepared under other conditions;
FIG. 5 is a field emission scanning electron microscope image of a sample prepared under other conditions;
FIG. 6 is a field emission scanning electron microscope image of a sample prepared under other conditions;
FIG. 7 shows the SERS substrate of FIG. 1 as a flexible transparent substrate, at 10 -6 (mol/l) Raman spectra at different positions in ATP solution;
FIG. 8 is a flow chart of the steps of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 8, the step flow of the SERS substrate constructed by the flexible transparent cone ordered array is described in detail in examples 1-6, experimental articles and equipment: PI (polyimide film), reactive ion etcher, plasma magnetron sputtering coating instrument, ultrasonic cleaner, ultra-pure water machine and SF 6 Gas, O 2 。
Example 1
The experimental steps are as follows:
(1) Firstly, performing ultrasonic cleaning on the sheared PI (polyimide film) film, preparing PS sphere liquid with the specification of 500nm, and after the film is cleaned and dried, keeping the film for later use.
(2) And (3) transferring the PS balls to the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI paved with PS balls, wherein the gas is sulfur hexafluoride (SF 6 ) And oxygen (O) 2 ) Wherein SF is 6 Flow rate is 40sccm, O 2 The flow rate was 20sccm.
(4) The power used for reactive ion etching was 150W.
(5) Performing magnetron sputtering plating (Au, ag) on the etched PI, and finally selecting after multiple tests; au was plated for 50 seconds and Ag was plated for 100 seconds.
(6) And observing the experimental PI under a scanning electron microscope to obtain a nanostructure image, as shown in figure 1.
In FIG. 1, SF is performed using 500nm PS balls as a mask 6 Flow rate is 40sccm, O 2 The flow is 20sccm, the power of the reactive ion etcher is 150W, the etching time is 180 seconds, and the plating is that Au is plated for 50 seconds and Ag is plated for 100 seconds;
(7) Immersing the sample etched for 180 seconds in 10 -6 Raman spectra at various positions in (mol/l) 4-ATP solution are shown in FIG. 7.
Example 2
The experimental steps are as follows:
(1) Firstly, ultrasonic cleaning is carried out on the sheared PI (polyimide film) film, meanwhile, PS ball liquid with the specification of 500nm is prepared, and the film is ready for use after cleaning and drying are finished.
(2) And (3) transferring the PS balls to the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI paved with PS balls, wherein the gas is sulfur hexafluoride (SF 6 ) And oxygen (O) 2 ) Wherein SF is 6 Flux is 40sccm, O 2 The flux was 20ccm, the reactive ion etcher power was 150W, and the etching times were 120 seconds, respectively.
(4) The power used for reactive ion etching was 150W.
(5) And (3) performing magnetron sputtering plating (Au and Ag) on the etched PI, wherein Au is plated for 50 seconds and Ag is plated for 100 seconds.
(6) And observing the experimental PI under a scanning electron microscope to obtain a nanostructure image, as shown in figure 2.
In fig. 2, the preparation conditions are: SF with 500nm PS balls as mask 6 Flow rate is 40sccm, O 2 The flow is 20sccm, the power of the reactive ion etcher is 150W, the etching time is 120 seconds, and the plating is that Au is plated for 50 seconds and Ag is plated for 100 seconds;
example 3
The experimental steps are as follows:
(1) Firstly, ultrasonic cleaning is carried out on the sheared PI (polyimide film) film, meanwhile, PS ball liquid with the specification of 500nm is prepared, and the film is ready for use after cleaning and drying are finished.
(2) And (3) transferring the PS balls to the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI paved with PS balls, wherein the gas is sulfur hexafluoride (SF 6 ) And oxygen (O) 2 ) Wherein SF is 6 Flux is 40sccm, O 2 The flux was 20ccm, the reactive ion etcher power was 150W, and the etching times were 60 seconds, respectively.
(4) The power used for reactive ion etching was 150W.
(5) And (3) performing magnetron sputtering plating (Au and Ag) on the etched PI, wherein Au is plated for 50 seconds and Ag is plated for 100 seconds.
(6) And observing the experimental PI under a scanning electron microscope to obtain a nanostructure image, as shown in figure 3.
In fig. 3, the preparation conditions are: SF with 500nm PS balls as mask 6 Flow rate is 40sccm, O 2 The flow is 20sccm, the power of the reactive ion etcher is 150W, the etching time is 60 seconds, and the plating is that Au is plated for 50 seconds and Ag is plated for 100 seconds.
Example 4
The experimental steps are as follows:
(1) Firstly, ultrasonic cleaning is carried out on the sheared PI (polyimide film) film, meanwhile, PS ball liquid with the specification of 500nm is prepared, and the film is ready for use after cleaning and drying are finished.
(2) And (3) transferring the PS balls to the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI paved with PS balls, wherein the gas is sulfur hexafluoride (SF 6 ) And oxygen (O) 2 ) Wherein SF is 6 Flux is 60sccm, O 2 The 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) performing magnetron sputtering plating (Au and Ag) on the etched PI, wherein Au is plated for 50 seconds and Ag is plated for 100 seconds.
(6) And observing the experimental PI under a scanning electron microscope to obtain a nanostructure image, as shown in figure 4.
In FIG. 4The preparation conditions are as follows: SF (sulfur hexafluoride) 6 Flow is 60sccm, O 2 The flow is 20sccm, the power of the reactive ion etcher is 180W, and the etching time is 180 seconds respectively; the plating is to plate Au for 50 seconds and then Ag for 100 seconds.
Example 5
The experimental steps are as follows:
(1) Firstly, ultrasonic cleaning is carried out on the sheared PI (polyimide film) film, meanwhile, PS ball liquid with the specification of 500nm is prepared, and the film is ready for use after cleaning and drying are finished.
(2) And (3) transferring the PS balls to the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI paved with PS balls, wherein the gas is sulfur hexafluoride (SF 6 ) And oxygen (O) 2 ) Wherein SF is 6 Flux is 60sccm, O 2 The flux was 20sccm, the reactive ion etcher power was 180W, and the etching times were 120 seconds, respectively.
(4) The power used for reactive ion etching was 180W.
(5) And (3) performing magnetron sputtering plating (Au and Ag) on the etched PI, wherein Au is plated for 50 seconds and Ag is plated for 100 seconds.
(6) And observing the experimental PI under a scanning electron microscope to obtain a nanostructure image, as shown in figure 5.
In fig. 5, the preparation conditions are: SF (sulfur hexafluoride) 6 Flow is 60sccm, O 2 The flow is 20sccm, the power of the reactive ion etcher is 180W, and the etching time is 120 seconds respectively; the plating is to plate Au for 50 seconds and then Ag for 100 seconds.
Example 6
The experimental steps are as follows:
(1) Firstly, ultrasonic cleaning is carried out on the sheared PI (polyimide film) film, meanwhile, PS ball liquid with the specification of 500nm is prepared, and the film is ready for use after cleaning and drying are finished.
(2) And (3) transferring the PS balls to the cleaned PI, and paving the PS balls on the surface of the PI for later use.
(3) Performing reactive ion etching on PI paved with PS balls, wherein the gas is sulfur hexafluoride (SF 6 ) And oxygen (O) 2 ) Wherein SF is 6 Flux of 60sccm，O 2 The flux was 20ccm, the reactive ion etcher power was 180W, and the etching times were 60 seconds, respectively.
(4) The power used for reactive ion etching was 180W.
(5) And (3) performing magnetron sputtering plating (Au and Ag) on the etched PI, wherein Au is plated for 50 seconds and Ag is plated for 100 seconds.
(6) And observing the experimental PI under a scanning electron microscope to obtain a nanostructure image, as shown in figure 6.
In FIG. 6, SF 6 Flow is 60sccm, O 2 The flow is 20sccm, the power of the reactive ion etcher is 180W, and the etching time is 60 seconds respectively; the plating is to plate Au for 50 seconds and then Ag for 100 seconds.
In summary, in FIG. 1, the cone-structured ordered array structure has a period of 500nm and the surface is roughened gold-silver nanoparticles. As can be seen from the two broken photographs in the figure, the cone is of hollow construction.
In FIG. 2, the ordered array structure is constructed like a cylinder, the period is 500nm, and the surface is rough gold and silver nano particles. The cylinder is of solid construction.
In FIG. 3, the cone-structured ordered array structure has a period of 500nm and a rough gold-silver nanoparticle surface. With respect to fig. 1, the cone is of solid construction and the cone is reduced in size.
In FIG. 4, the broken cylinders form an ordered array structure with a period of 500nm and rough gold and silver nanoparticles on the surface. With respect to fig. 2, the array is constructed as a broken hollow cylinder structure.
In FIG. 5, the broken cone is constructed into an ordered array structure with a period of 500nm and a rough gold-silver nanoparticle surface. With respect to fig. 1, the array is constructed as a broken hollow cone structure.
In FIG. 6, the cone-structured ordered array structure has a period of 500nm and a rough gold-silver nanoparticle surface. With respect to fig. 1 and 3, the cone is a solid structure and the surface is formed of nanowires.
FIG. 7 is a Raman spectrum obtained by using FIG. 1 as a substrate and 4-ATP as a probe molecule. With other substrates, raman spectra of 4-ATP could not be obtained under the same conditions. In summary, only in the case of example 1, a flexible transparent cone ordered array structure could be obtained, and this structure has better SERS performance.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the 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 scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. A preparation method of a SERS substrate constructed by a flexible transparent cone ordered array is characterized by comprising the following steps:
step 1, firstly, performing ultrasonic cleaning on a sheared PI film, and simultaneously preparing PS ball liquid with the specification of 500nm, and after the PI film is cleaned and dried, keeping the PI film for later use;
in the step 1, the thickness of the PI film is 20 mu m;
the PS balls with the specification of 500 and nm used in the step 1 are used as masks and are formed by changing experimental conditions in reactive ion etching;
step 2, PS ball transfer is carried out on the cleaned PI film, and PS balls are paved on the surface of the PI film for standby;
step 3, performing reactive ion etching on the PI film paved with the PS balls, wherein the gas is SF 6 And O 2 Wherein SF is 6 Flow rate is 40sccm, O 2 The flow rate is 20sccm;
in the step 3, the power used for reactive ion etching is 150W, and the etching time is 180s;
and 4, performing magnetron sputtering coating on the PI film etched by the reactive ions, wherein Au is firstly coated for 50s, and then Ag is coated for 100s.
2. The method for preparing the SERS substrate constructed by the flexible transparent cone ordered array according to claim 1, further comprising observing the experimental PI film under a scanning electron microscope to obtain a nanostructure image.
3. The method for preparing the SERS substrate constructed by the flexible transparent cone ordered array according to any one of claims 1-2, wherein the prepared SERS substrate is a flexible transparent substrate constructed by the hollow cone ordered array.
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