CN103674924A - Raman spectrum test probe and manufacturing method thereof - Google Patents
Raman spectrum test probe and manufacturing method thereof Download PDFInfo
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- CN103674924A CN103674924A CN201210338058.8A CN201210338058A CN103674924A CN 103674924 A CN103674924 A CN 103674924A CN 201210338058 A CN201210338058 A CN 201210338058A CN 103674924 A CN103674924 A CN 103674924A
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- 238000012360 testing method Methods 0.000 title claims abstract description 44
- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 41
- 239000000523 sample Substances 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 74
- 239000002184 metal Substances 0.000 claims abstract description 74
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000005498 polishing Methods 0.000 claims abstract description 13
- 238000005260 corrosion Methods 0.000 claims abstract description 8
- 230000007797 corrosion Effects 0.000 claims abstract description 8
- 239000013307 optical fiber Substances 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 229910052709 silver Inorganic materials 0.000 claims description 9
- 239000004332 silver Substances 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- 239000005304 optical glass Substances 0.000 claims description 4
- 238000001259 photo etching Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 12
- 238000001514 detection method Methods 0.000 abstract description 7
- 230000003287 optical effect Effects 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000005530 etching Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 230000000873 masking effect Effects 0.000 abstract 1
- 238000000772 tip-enhanced Raman spectroscopy Methods 0.000 description 16
- 229920002120 photoresistant polymer Polymers 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000010453 quartz Substances 0.000 description 7
- 238000001069 Raman spectroscopy Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 6
- 101000674278 Homo sapiens Serine-tRNA ligase, cytoplasmic Proteins 0.000 description 4
- 101000674040 Homo sapiens Serine-tRNA ligase, mitochondrial Proteins 0.000 description 4
- 102100040516 Serine-tRNA ligase, cytoplasmic Human genes 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000004621 scanning probe microscopy Methods 0.000 description 1
- 238000001845 vibrational spectrum Methods 0.000 description 1
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Abstract
The invention relates to the optical detection field, and discloses a Raman spectrum test probe. The Raman spectrum test probe comprises a substrate and a plurality of array nano metal columns, wherein the substrate test surface is a polished surface, and the array nano metal columns are arranged on the polished surface; the top of each of the array nano metal columns is of a tapered needle tip structure. The invention also discloses a method for manufacturing the Raman spectrum test probe. The method comprises the technological procedures of polishing, coating, masking, etching, corroding and mask removing, and the manufacturing cost is low. The TERS (Tip-enhanced Raman spectrum) technology-based Raman spectrum test probe provided by the invention is simple in structure, and in comparison with a probe with a single tip, the Raman spectrum test probe has bigger detection area and can be coupled with laser more conveniently; photolithographic mask and metal corrosion technologies are used for manufacturing the Raman spectrum test probe, so that the manufacturing cost is low, the shape of the array nano metal columns with tip structures is easy to control, and the distribution of the array nano metal columns is regular.
Description
Technical field
The present invention relates to optical detection field, relate in particular to a kind of Raman spectrum test probe and preparation method thereof.
Background technology
Raman spectrum is a kind of molecular vibration spectrum, can reflect the feature structure of molecule.Yet raman spectral signal is conventionally very weak, and its intensity only has 10 of incident intensity
-10.Therefore the detection of Raman spectrum, in concrete application, need to rely on certain enhancement effect to improve raman spectrum strength conventionally.
SERS(Surface-Enhanced Raman Scattering Surface enhanced raman spectroscopy) effect is exactly a kind of surface enhanced effect relevant to rough surface.The metals such as gold, silver, copper are carried out after surface roughening processing, and the raman spectral signal of its surface molecular can strengthen 6 orders of magnitude.Visible SERS effect can strengthen the Raman signal of surface molecular greatly.But this effect is only applicable to rough surface, for level and smooth single-crystal surface, its Raman signal cannot strengthen by SERS effect.
TERS(Tip-enhanced Raman spectroscopy Tip-Enhanced Raman Spectroscopy) effect is also a kind of surface enhancing technology of Raman spectrum.It is combined by scanning probe microscopy and Raman spectroscopy.TERS technology can realize ganoid and not possess the research of the material of SERS activity, but also can obtain very high spatial resolution.Yet because TERS technology is the combination of scan-probe fibre technology and Raman spectroscopy, it has brought following difficult point to the research of TERS technology: how (1) sets up stable TERS system; (2) how to obtain most advanced and sophisticated littlely, tapering is little, surface-brightening and the active needle point of the high TERS polluting without carbon species; (3) in TERS testing process, how to avoid needle point not contaminated; (4) incident realizes the quick and precisely coupling of laser facula and TERS needle point etc.These difficult points are brought very large difficulty to the research of TERS technology and the popularization of application.
Summary of the invention
For the problems referred to above, the present invention proposes a kind of based on TERS(Tip-Enhanced Raman Spectroscopy) the Raman spectrum test probe of technology and preparation method thereof, simple in structure, cost of manufacture is low, has the larger detection total area, with laser coupled more convenient and quicker.
For achieving the above object, the technical scheme that the present invention proposes is: a kind of Raman spectrum test probe, comprise substrate and array nano metal column, and described substrate test surfaces is polished surface, array nano metal column is located on this polished surface; Each column top of described array nano metal column is the needle point structure with tapering.
Further, more than the face shape of described polished surface within the scope of final effective aperture of using reaches λ/100.
Further, described substrate is multimode optical fiber or optical glass.
Further, described array nano metal stud materials is gold, silver or copper.
The method for making of above-mentioned Raman spectrum test probe, comprises the steps: 1) substrate polishing, substrate test surfaces is carried out to polishing, more than effective coverage inner face shape reaches λ/100; 2) metal-coated membrane, metal-coated membrane on the polished surface of substrate, thickness of metal film is at 100nm ~ 500nm; 3) scribe mask layer, on metal film, be coated with last layer mask layer, and mask layer is carried out to photoetching treatment formation mask array pillar construction; 4) corroding metal film, metallic diaphragm is carried out to corrosion processing, form the array nano metal column corresponding with mask layer, by controlling technological parameter, as photoresist mask layer thickness or corrosive liquid concentration etc., make each column top of array nano metal column form the needle point structure with tapering; 5) remove mask layer, by remaining mask layer eccysis.
Further, the array of mask described in step 3) column dutycycle is 0.3 ~ 0.7.
Further, step 2), thickness of metal film is at 100nm ~ 200nm.
Further, the material of described metal film is gold, silver or copper.
Further, described substrate is multimode optical fiber or optical glass.
Beneficial effect of the present invention is: the Raman spectrum test probe that the present invention is based on TERS technology is simple in structure, and with respect to the probe of single needle point, its detection area is larger, and more aspect is quick with laser coupled; Adopt photo etched mask and metal erosion technique to make above-mentioned Raman spectrum test probe, cost of manufacture is low, and the shape of the array nano metal column of tool needle point structure is easy to control, and the regularity of distribution.
Accompanying drawing explanation
Fig. 1 is Raman spectrum test probe embodiment of the present invention mono-structural representation;
Fig. 2 is Raman spectrum test probe embodiment of the present invention bis-structural representations;
Fig. 3 is Raman spectrum test probe embodiment mono-manufacturing process schematic diagram of the present invention;
Fig. 4 is Raman spectrum test probe embodiment bis-manufacturing process schematic diagram of the present invention.
Reference numeral: 1, array nano metal column; 101, metal film; 2, multimode optical fiber substrate; 3, quartz substrate; 4, mask array column; 401, mask layer.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Of the present invention based on TERS(Tip-Enhanced Raman Spectroscopy) the Raman spectrum test probe of technology, comprise substrate and array nano metal column, wherein substrate test surfaces is polished surface, array nano metal column is located on this polished surface; Each column top of array nano metal column is the needle point structure with tapering.
Concrete, embodiment mono-as shown in Figure 1, adopt multimode optical fiber as substrate, these multimode optical fiber substrate 2 end faces are carried out to polishing, more than polished surface shape is controlled at λ/100, be distributed with array nano metal column 1 on polished surface, each column top is the needle point structure with tapering, array nano metal column 1 in this embodiment is to be made by mask corrosion by the thick metal film of 200nm, and its array dutycycle is 0.3.Wherein, array nano metal column 1 material can adopt the transition metal such as gold, silver or copper.By the other end of this multimode optical fiber substrate 2 and Raman spectrum Laser output fused fiber splice, this Raman spectrum test probe can be realized the detection of flashlight and the transmission of incoming signal light and detectable signal light, and this Raman spectrum test probe can be surveyed for the Raman spectrum of liquid, gas and optical surface.
If Fig. 2 is the embodiment bis-of Raman spectrum test probe, adopt quartzy as substrate, the size of quartz substrate 3 can be selected according to the laser facula size in reality use, in this embodiment, quartz substrate 3 is of a size of 1mm * 1mm * 1mm, the searching surface of quartz substrate 3 is carried out to polishing, more than polished surface shape is controlled at λ/100.On polished surface, be distributed with array nano metal column 1, each column top is the needle point structure with tapering, and the array nano metal column 1 in this embodiment is to be made by mask corrosion by the thick metal film of 100nm, and its array dutycycle is 0.4.Wherein, array nano metal column 1 material can adopt the transition metal such as gold, silver or copper.
The method for making of above-mentioned Raman spectrum test probe comprises the technique processes such as polishing, plated film, mask, etching, corrosion and removal mask, and cost of manufacture is low.
Concrete, the manufacturing process of Raman spectrum test probe in embodiment mono-as shown in Figure 3, comprise the steps: 1) substrate polishing, multimode optical fiber substrate 2 test surfaces are carried out to polishing, more than effective coverage inner face shape reaches λ/100, can first multimode optical fiber be inserted in quartz glass capillary, then the polishing of one-tenth dish; 2) metal-coated membrane, on the polished surface of multimode optical fiber substrate 2, metal-coated membrane 101, and metal film 101 thickness are in 200nm left and right; 3) scribe mask layer 401, on metal film 101, be coated with last layer photoresist mask layer 401, its THICKNESS CONTROL is below 1 micron, and photoresist mask layer 401 is carried out to photoetching treatment, on metal film 101, form mask array column 4 structures, realize the mask pattern of array column, its dutycycle is 0.3; 4) corroding metal film 101, by chemistry or electrochemical reaction, metal film 101 is carried out to corrosion processing, by the graph copying of mask array column 4 in metal film 101, form the array nano metal column 1 corresponding with mask array column 4, and by controlling technological parameter, as photoresist mask layer thickness, corrosive liquid concentration etc., make array nano metal column 1 each column top form the needle point structure with tapering; 5) remove mask layer 401, by remaining photoresist mask layer eccysis, realize the array nano metal column 1 of producing on multimode optical fiber substrate 2 end faces.In this embodiment, what metal membrane material adopted is gold, also can adopt other transition metal materials such as silver or copper.Wherein, array dutycycle should consider in conjunction with metal film 101 thickness and corrosive liquid performance.Wherein, the face shape of λ/100 refers to the face shape within the scope of the effective aperture of finished product.For substrate, be multimode optical fiber scheme, its effective coverage scope, is multimode optical fiber end face, and as the circle of diameter 0.25mm, the round inner face shape at diameter 0.25 need to reach λ/100.
As shown in Figure 4 be the manufacturing process of the Raman spectrum test probe in embodiment bis-, comprise the steps: 1) substrate polishing, extract the quartzy plain film of a 10mm * 10mm * 1mm as substrate, these quartz substrate 3 test surfaces are carried out to polishing, more than effective coverage inner face shape reaches λ/30; 2) metal-coated membrane 101, and on the polished surface of quartz substrate 3, metal-coated membrane 101, and metal film 101 thickness are in 100nm left and right; 3) scribe mask layer 401, on metal film 101, be coated with last layer photoresist mask layer 401, its THICKNESS CONTROL is below 1 micron, and photoresist mask layer 401 is carried out to photoetching treatment, on metal film 101, form mask array column 4 structures, realize the mask pattern of array column, its dutycycle is 0.4; 4) corroding metal film 101, by chemistry or electrochemical reaction, metal film 101 is carried out to corrosion processing, by the graph copying of mask array column 4 in metal film 101, form the array nano metal column 1 corresponding with mask array column 4, and by controlling technological parameter, as photoresist mask layer thickness, corrosive liquid concentration etc., make array nano metal column 1 each column top form the needle point structure with tapering; 5) remove mask layer 401, by remaining photoresist mask layer eccysis, realize the array nano metal column 1 of producing on quartz substrate 3 end faces; 6) according to actual user demand, the product of 10mm*10mm*1mm is cut, as be cut into 1mm*1mm*1mm etc., obtain the test surfaces of face shape more than λ/100.In this embodiment, what metal membrane material adopted is silver, also can adopt other transition metal materials such as gold or copper.Wherein, array dutycycle should consider in conjunction with metal film 101 thickness and corrosive liquid performance.
Although specifically show and introduced the present invention in conjunction with preferred embodiment; but those skilled in the art should be understood that; within not departing from the spirit and scope of the present invention that appended claims limits; the various variations of in the form and details the present invention being made, are protection scope of the present invention.
Claims (9)
1. a Raman spectrum test probe, comprises substrate and array nano metal column, it is characterized in that: described substrate test surfaces is polished surface, and array nano metal column is located on this polished surface; Each column top of described array nano metal column is the needle point structure with tapering.
2. a kind of Raman spectrum test probe as claimed in claim 1, is characterized in that: more than the face shape of described polished surface in effective usable range reaches λ/100.
3. a kind of Raman spectrum test probe as claimed in claim 1, is characterized in that: described substrate is multimode optical fiber or optical glass.
4. a kind of Raman spectrum test probe as claimed in claim 1, is characterized in that: described array nano metal stud materials is gold, silver or copper.
5. a method for making for Raman spectrum test probe, is characterized in that: comprise the steps: 1) substrate polishing, substrate test surfaces is carried out to polishing, more than effective coverage inner face shape reaches λ/100; 2) metal-coated membrane, metal-coated membrane on the polished surface of substrate, thickness of metal film is at 100nm ~ 500nm; 3) scribe mask layer, on metal film, be coated with last layer mask layer, and mask layer is carried out to photoetching treatment formation mask array pillar construction; 4) corroding metal film, carries out corrosion processing to metallic diaphragm, forms the array nano metal column corresponding with mask layer, by controlling technological parameter, makes each column top of array nano metal column form the needle point structure with tapering; 5) remove mask layer, by remaining mask layer eccysis.
6. a kind of method for making of Raman spectrum test probe as claimed in claim 5, is characterized in that: the array of mask described in step 3) column dutycycle is 0.3 ~ 0.7.
7. a kind of method for making of Raman spectrum test probe as claimed in claim 5, is characterized in that: step 2) in thickness of metal film at 100nm ~ 200nm.
8. a kind of method for making of Raman spectrum test probe as claimed in claim 5, is characterized in that: the material of described metal film is gold, silver or copper.
9. a kind of method for making of Raman spectrum test probe as claimed in claim 5, is characterized in that: described substrate is multimode optical fiber or optical glass.
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| CN201210338058.8A CN103674924A (en) | 2012-09-13 | 2012-09-13 | Raman spectrum test probe and manufacturing method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104267020A (en) * | 2014-10-28 | 2015-01-07 | 首都师范大学 | Optical fiber raman radar and design method thereof |
| CN106596509A (en) * | 2016-12-29 | 2017-04-26 | 天津大学 | Portable raman-microscratch rapid detector integrated with wireless data transmission function |
| CN111362225A (en) * | 2020-03-17 | 2020-07-03 | 中国科学院半导体研究所 | Nano needle tip structure, composite structure and preparation method thereof |
| CN114814314A (en) * | 2022-04-18 | 2022-07-29 | 苏州伊欧陆系统集成有限公司 | Multi-contact high-current high-voltage test probe |
| CN118191384A (en) * | 2022-12-14 | 2024-06-14 | 上海泽丰半导体科技有限公司 | Linear probe and method for manufacturing the same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106596509A (en) * | 2016-12-29 | 2017-04-26 | 天津大学 | Portable raman-microscratch rapid detector integrated with wireless data transmission function |
| CN111362225A (en) * | 2020-03-17 | 2020-07-03 | 中国科学院半导体研究所 | Nano needle tip structure, composite structure and preparation method thereof |
| CN111362225B (en) * | 2020-03-17 | 2024-01-30 | 中国科学院半导体研究所 | Nano needle point structure, composite structure and preparation method thereof |
| CN114814314A (en) * | 2022-04-18 | 2022-07-29 | 苏州伊欧陆系统集成有限公司 | Multi-contact high-current high-voltage test probe |
| CN114814314B (en) * | 2022-04-18 | 2024-02-13 | 苏州伊欧陆系统集成有限公司 | Multi-contact high-current high-voltage test probe |
| CN118191384A (en) * | 2022-12-14 | 2024-06-14 | 上海泽丰半导体科技有限公司 | Linear probe and method for manufacturing the same |
| CN118191384B (en) * | 2022-12-14 | 2024-10-01 | 上海泽丰半导体科技有限公司 | Linear probe and method for manufacturing the same |
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Application publication date: 20140326 |