CN108996469A - A kind of silicon substrate of the production method and application of nano-hole golden the film film - Google Patents
A kind of silicon substrate of the production method and application of nano-hole golden the film film Download PDFInfo
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- CN108996469A CN108996469A CN201810839588.8A CN201810839588A CN108996469A CN 108996469 A CN108996469 A CN 108996469A CN 201810839588 A CN201810839588 A CN 201810839588A CN 108996469 A CN108996469 A CN 108996469A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
- B81C1/00373—Selective deposition, e.g. printing or microcontact printing
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Abstract
The invention discloses the silicon substrates of a kind of production method of nano-hole golden film and the application film, including silicon wafer to be processed, the production method of micro-structure nano-hole golden film on the surface of silicon wafer the following steps are included: make to form uniform single layer polystyrene microsphere layer, the diameter of polystyrene microsphere is reduced using oxygen plasma, guarantee microballoon gap, micro-structure is etched on silicon wafer, polystyrene microsphere layer is removed to the machined surface of silicon wafer, form silicon substrate, in one layer of electrum film of silicon substrate surface uniform fold, by the silver atoms removal in electrum film, form micro-structure nano-hole golden film.The beneficial effects of the invention are as follows, by forming polystyrene microsphere layer on the surface of silicon wafer, then go out the method for different silicon substrate surface micro-structures by reactive ion etching in silicon substrate surface, hole gold thin film is laid on to the silicon substrate surface of different micro-structures, by relatively can be easy obtain the optimal hole gold thin film structure for raman spectroscopy measurement.
Description
Technical field
The present invention relates to semiconductor field, the silicon of the production method and application of especially a kind of nano-hole golden film film
Base.
Background technique
Surface plasma metal nanoparticle has huge potentiality in fields such as sensing, photovoltaic, development and biologic medicals.
Mat gold (nano-hole golden) material with nanovoids is obtained because of its unique three-dimensional co-continuous nanostructure among these
Obtained extensive concern.However, nano-pore gold bullion and nano-pore golden film have attribute non-adjustable, Surface Raman Spectra characterization is weak
The defects of.
Summary of the invention
The purpose of the present invention is to solve the above problems, devise the production method and application of a kind of nano-hole golden film
The silicon substrate of the film.
Realize above-mentioned purpose the technical scheme is that, a kind of production method of nano-hole golden film and apply the film
Silicon substrate, including silicon wafer to be processed, the production method of micro-structure nano-hole golden film the following steps are included:
A, it makes to form uniform single layer polystyrene microsphere layer on the surface of silicon wafer.
B, the diameter of polystyrene microsphere is reduced using oxygen plasma, guarantees microballoon gap.
C, micro-structure is etched on silicon wafer.
D, polystyrene microsphere layer is removed to the machined surface of silicon wafer, forms silicon substrate.
E, in one layer of electrum film of silicon substrate surface uniform fold.
F, the silver atoms in electrum film are removed, forms micro-structure nano-hole golden film.
In step a, the method that silicon chip surface forms single layer polystyrene microsphere layer uses Langmuir-Blodgett
trough。
In step c, silicon chip etching uses reactive ion etching (RIE) technology, chooses CF4 (carbon tetrafluoride) as erosion
Carve gas.
In step d, remaining polystyrene microsphere is removed from silicon substrate surface using chloroform solvent.
It is thin in silicon substrate surface one laminated gold of covering using electrum target by sputter coating technology in step e
Film.
Gold and silver atom number ratio is 28:72 in the electrum target.
In step f, the method that silver atoms in electrum film are removed is to be put in the de- conjunction impregnated in concentrated nitric acid
Gold process.
The concentration of the concentrated nitric acid is 68%.
Application response ion(ic) etching (RIE) technology, choosing CF4 (carbon tetrafluoride) is etching gas, by accurately controlling erosion
Power, time, etching air pressure are carved, a variety of micro-structures may be implemented.
The etching power, time, etching air pressure, and the corresponding a variety of micro-structures realized specifically,
Etching power 100W, etching period 3min etch air pressure 10mtorr, and silicon substrate surface micro-structure is disk-like structure,
Etching power 100W, etching period 6min etch air pressure 20mtorr, and silicon substrate surface micro-structure is pyramidal structure,
Etching power 100W, etching period 6min, etch air pressure 100mtorr, and silicon substrate surface micro-structure is acicular texture.
The beneficial effect is that then being passed through in silicon substrate surface by forming polystyrene microsphere layer on the surface of silicon wafer
Hole gold thin film is laid on the silicon substrate table of different micro-structures by the method that reactive ion etching goes out different silicon substrate surface micro-structures
Face, by relatively can be easy obtain the optimal hole gold thin film structure for raman spectroscopy measurement.
Detailed description of the invention
Fig. 1 is a kind of production method of nano-hole golden film of the present invention and the production method of the silicon substrate using the film
Step abcef process schematic；
Fig. 2 be a kind of nano-hole golden film of the present invention production method and application the film silicon substrate plate-like, cone
The corresponding cef process micro-structure diagram of shape, needle-shaped silicon substrate；
Fig. 3 be a kind of nano-hole golden film of the present invention production method and application the film silicon substrate plate-like, cone
Shape, acicular microstructure carry out raman spectroscopy measurement comparative result figure；
Specific embodiment
The present invention is specifically described with reference to the accompanying drawing, as shown in Figs. 1-2, a kind of production side of nano-hole golden film
The silicon substrate of method and the application film, including silicon wafer to be processed, the production method of micro-structure nano-hole golden film includes following step
It is rapid:
A, it makes to form uniform single layer polystyrene microsphere layer on the surface of silicon wafer, single layer polystyrene microsphere layer is used for
The surface of silicon wafer is not influenced by etching gas where protecting microballoon layer.
B, the diameter of polystyrene microsphere is reduced using oxygen plasma, guarantees microballoon gap, and the gap size of microballoon is straight
Connecing influences the micro-structure that subsequent silicon chip etching goes out.
C, micro-structure is etched on silicon wafer, etches different micro-structures by controlling etching condition.
D, polystyrene microsphere layer is removed to the machined surface of silicon wafer, silicon substrate is formed, has formed the micro-structure of needs, polyphenyl
Ethylene microballoon layer is ineffective, removes it, and prepares for subsequent step.
E, in one layer of electrum film of silicon substrate surface uniform fold, electrum overall film thickness is 50-200nm.
F, the silver atoms in electrum film are removed, forms micro-structure nano-hole golden film, the silver in electrum
Atom is by being chemically removed, and the position where silver atoms is substituted by cavity before, and the position of gold atom is constant, and formation has
Porous golden film, i.e. hole gold thin film；
In step a, the method that silicon chip surface forms single layer polystyrene microsphere layer uses Langmuir-Blodgett
trough；
In step c, silicon chip etching uses reactive ion etching (RIE) technology, chooses CF4 (carbon tetrafluoride) as erosion
Gas is carved, which can be chemically reacted with silicon wafer, the region for not having coverlet strata phenylethylene micro ball to cover silicon chip surface
It etches away, to macroscopically form micro-structure in silicon chip surface；
In step d, remaining polystyrene microsphere is removed from silicon substrate surface using chloroform solvent, polystyrene microsphere
Layer is for protecting silicon wafer from the etching of CF4 gas, and polystyrene is just ineffective after the silicon substrate of micro-structure is formed, and is moved
It removes；
It is thin in silicon substrate surface one laminated gold of covering using electrum target by sputter coating technology in step e
Film；
Gold and silver atom number ratio is 28:72 in the electrum target；
In step f, the method that silver atoms in electrum film are removed is to be put in the de- conjunction impregnated in concentrated nitric acid
Gold process, silver is reacted with concentrated nitric acid generates silver nitrate, so that silver atoms be removed, it is thin that the gold not reacted with concentrated nitric acid forms hole gold
Film；
The concentration of the concentrated nitric acid is 68%；
Application response ion(ic) etching (RIE) technology, choosing CF4 (carbon tetrafluoride) is etching gas, by accurately controlling erosion
Power, time, etching air pressure are carved, a variety of micro-structures may be implemented,
The etching power, time, etching air pressure, and the corresponding a variety of micro-structures realized specifically,
Etching power 100W, etching period 3min etch air pressure 10mtorr, and silicon substrate surface micro-structure is disk-like structure,
Etching power 100W, etching period 6min etch air pressure 20mtorr, and silicon substrate surface micro-structure is pyramidal structure,
Etching power 100W, etching period 6min, etch air pressure 100mtorr, and silicon substrate surface micro-structure is acicular texture；
As shown in figure 3, Fig. 3 indicates that micro-structure nano-hole golden film after processing is completed has carried out Surface enhanced Raman spectroscopy
Characterization, the monofilm for choosing benzenethiol are to characterize molecule, the Surface enhanced Raman spectroscopy of acquisition, it can be seen from the figure that
Raman substrate with arbitrary surfaces micro-structure, Raman Characterization are more excellent than the Raman substrate measurement effect of no micro-structure
It is different, and can see acicular microstructure is the Raman spectrum reinforcing effect that nano-hole golden film brings 5 times or more.
Working principle:
As shown in Figs. 1-2, step a covers one layer by Langmuir-Blodgett trough technology in silicon chip surface
Polystyrene microsphere layer, the surface of silicon wafer is not by subsequent step c where single layer polystyrene microsphere layer is used to protect microballoon layer
Etching gas influences, step b, and the diameter of polystyrene microsphere is reduced using oxygen plasma, guarantees microballoon gap, between microballoon
Gap size directly affects the micro-structure that subsequent silicon chip etching goes out, step c, by different silicon chip etchings at different micro-structures, silicon wafer
Etching uses reactive ion etching (RIE) technology, chooses CF4 (carbon tetrafluoride) and is used as etching gas, by controlling the reaction
Etching power, time, etching air pressure in journey is to be etched into the micro-structures such as disk dress, taper, needle-shaped (as shown in Fig. 2, picture is left
Side is successively disk dress, taper, acicular microstructure from top to bottom), step d, using chloroform solvent by remaining polystyrene microsphere from
Silicon substrate surface removes (Fig. 1 omits the step), step e, by sputter coating technology, using electrum target in silicon substrate surface
A laminated gold thin film is covered, the structure of the alloy firm is identical as the silicon substrate surface micro-structure that it is covered (as shown in Fig. 2, figure
It is successively the disk dress for covering electrum film, taper, needle-shaped substrate micro-structure from top to bottom among piece), step f passes through
The de- alloying technology that electrum is impregnated with concentrated nitric acid removes the silver atoms in electrum film, forms micro-structure nanometer
Hole gold thin film (as shown in Fig. 2, being successively disk dress, taper, the micro-structure hole gold thin film of needle-shaped substrate from top to bottom on the right side of picture).
Above-mentioned technical proposal only embodies the optimal technical scheme of technical solution of the present invention, those skilled in the art
The principle of the present invention is embodied to some variations that some of them part may be made, belongs to the scope of protection of the present invention it
It is interior.
Claims (10)
1. the silicon substrate of the production method and application of a kind of nano-hole golden film film, including silicon wafer to be processed, feature exists
In, micro-structure nano-hole golden film production method the following steps are included:
A, it makes to form uniform single layer polystyrene microsphere layer on the surface of silicon wafer.
B, the diameter of polystyrene microsphere is reduced using oxygen plasma, guarantees microballoon gap.
C, micro-structure is etched on silicon wafer.
D, polystyrene microsphere layer is removed to the machined surface of silicon wafer, forms silicon substrate.
E, in one layer of electrum film of silicon substrate surface uniform fold.
F, the silver atoms in electrum film are removed, forms micro-structure nano-hole golden film.
2. the silicon substrate of the production method and application of a kind of nano-hole golden film according to claim 1 film, in the step
In rapid a, which is characterized in that the method that silicon chip surface forms single layer polystyrene microsphere layer uses Langmuir-Blodgett
trough。
3. the silicon substrate of the production method and application of a kind of nano-hole golden film according to claim 1 film, in the step
In rapid c, which is characterized in that silicon chip etching uses reactive ion etching technique, chooses CF4 as etching gas.
4. the silicon substrate of the production method and application of a kind of nano-hole golden film according to claim 1 film, in the step
In rapid d, which is characterized in that removed remaining polystyrene microsphere from silicon substrate surface using chloroform solvent.
5. the silicon substrate of the production method and application of a kind of nano-hole golden film according to claim 1 film, in the step
In rapid e, which is characterized in that by sputter coating technology, cover a laminated gold thin film in silicon substrate surface using electrum target.
6. the silicon substrate of the production method and application of a kind of nano-hole golden film according to claim 4 film, feature
It is, gold and silver atom number ratio is 28:72 in the electrum target.
7. the silicon substrate of the production method and application of a kind of nano-hole golden film according to claim 1 film, in the step
In rapid f, which is characterized in that the method for removing silver atoms in electrum film is to be put in the de- alloy work impregnated in concentrated nitric acid
Skill.
8. the silicon substrate of the production method and application of a kind of nano-hole golden film according to claim 6 film, feature
It is, the concentration of the concentrated nitric acid is 68%.
9. a kind of silicon substrate of application micro-structure nano-hole golden film, which is characterized in that application response ion etching technology is chosen
CF4 is etching gas, and by accurately controlling etching power, time, etching air pressure, a variety of micro-structures may be implemented.
10. a kind of silicon substrate of application according to claim 9 micro-structure nano-hole golden film, which is characterized in that described
Etching power, time, etching air pressure, and the corresponding a variety of micro-structures realized specifically,
Etching power 100W, etching period 3min etch air pressure 10mtorr, and silicon substrate surface micro-structure is disk-like structure,
Etching power 100W, etching period 6min etch air pressure 20mtorr, and silicon substrate surface micro-structure is pyramidal structure,
Etching power 100W, etching period 6min, etch air pressure 100mtorr, and silicon substrate surface micro-structure is acicular texture.
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Cited By (4)
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| CN110726711A (en) * | 2019-10-29 | 2020-01-24 | 江南大学 | SERS substrate of metal-modified semiconductor-based bionic compound eye bowl structure and construction method |
| CN110735131A (en) * | 2019-10-29 | 2020-01-31 | 江南大学 | Bionic SERS substrate with metal-based compound eye bowl structures, construction method and application |
| CN111816558A (en) * | 2019-04-12 | 2020-10-23 | 中国科学院长春光学精密机械与物理研究所 | Method for manufacturing silicon-based deep hole microstructure |
| CN113702354A (en) * | 2021-09-02 | 2021-11-26 | 电子科技大学 | Flexible SERS substrate based on array type microstructure and preparation method thereof |
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| CN113702354A (en) * | 2021-09-02 | 2021-11-26 | 电子科技大学 | Flexible SERS substrate based on array type microstructure and preparation method thereof |
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