CN106989969A - A kind of tilted metallic nanostructured and preparation method thereof - Google Patents
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Abstract
The invention discloses a kind of tilted metallic nanostructured and preparation method thereof, prepared by the tilted metallic nanostructured is with polystyrene sphere template, a part for the metal material of deposition is raised by deposition of insulative material, makes entirely to deposit the certain inclination angle of obtained metal structure generation by metal material；The circular dichroism of the structure can be obtained using normal incidence method, and after the sedimentation time of increase deposition of insulative material, can obtain enhanced circular dichroism signal；The method that the present invention prepares incline structure compares the method for preparing incline structure using technologies such as electron beam lithography and laser direct-writings and has step simple, the saving time, and the characteristics of controllability is strong, meanwhile, the incline structure prepared using the method for the present invention is also applicable as strengthening the senser element of chiral molecules chiral information.
Description
Technical field
The invention belongs to metal Nano structure preparing technical field, and in particular to a kind of tilted metallic nanostructured and its system
Preparation Method.
Background technology
A chiral etymology represents the symmetry of structure, there is important meaning in a variety of subjects in Greek.If certain
Object is different from its mirror image, then it is referred to as " chiral ", and its mirror image can not be overlapped with the original, just as left hand with
The right hand each other mirror image and can not overlap.Chirality is the essential characteristic of life process, and the organic molecule for constituting life entity is most
All it is chiral molecules.
According to disclosed technology, circular dichroism (CD, circular dichroism) is research chipal compounds one
Individual highly important means, Cotton effect (Cotton Effect) at specific wavelengths it is positive and negative left and right with optical rotatory spectrum
Rotation is the same, and the macroscopic view mark of chiral enantiomer has equivalent effect, and can pass through the absolute of some regular chiral enantiomers
Configuration is judged.
The chiral structure of naturally occurring, circular dichroism is weaker, is unfavorable for widely application.Because metal and light have more
Strong interaction, metal Nano structure has stronger circular dichroism, therefore, is generally increased by preparing metal Nano structure
Its strong circular dichroism.
For the preparation of planar chiral metal structure and multilayer chiral metal nanostructured, electron beam can be generally used
Etch (T. Narushima, S. Hashiyada, and H. Okamoto. Nanoscopic study on
developing optical activity with increasing chirality for two-dimensional
Metal nanostructures. ACS photonics, 1 (8), 732-738 (2014)) and laser writing technology (A.
G. Poleshchuk, V. P. Korolkov. Laser writing systems and technologies for
fabrication of binary and continuous relief diffractive optical elements[C]//
International Conference on Lasers, Applications, and Technologies' 07.
International Society for Optics and Photonics: 67320X-67320X-10 (2007).2)。
But there is very big difficulty in operation and preparation technology when preparing tilted metallic nanostructured in these methods,
And waste time and energy, expense is also relatively expensive；Also, both technologies need also exist for using deposition step, and they prepare
The effective area of sample out is limited, and the work of this spectra collection to after proposes very big challenge, it is necessary to more
Many energy is debugged with the time can just measure signal.
The content of the invention
The electron beam lithography and laser writing technology that use are prepared in order to solve tilted metallic nanostructured in the prior art
The problem of existing, the invention provides a kind of method for preparing tilted metallic nanostructured, by being sunk on polystyrene sphere
Accumulate insulating materials to raise a part for the metal material of deposition, make whole metal Nano structure run-off the straight.Entirely deposited
Journey eliminates the complex steps of electron beam lithography machine laser direct-writing etc., and only needs simple three step, deposits two kinds of materials, it is possible to
Obtain inclined metal Nano structure, and change the sedimentation time of deposition of insulative material that metal Nano structure can also be changed
Inclined degree, strengthens corresponding circular dichroism signal.
The technical problem to be solved in the present invention is achieved through the following technical solutions：
A kind of tilted metallic nanostructured, the structure is deposited on the surface of polystyrene sphere, by the first metal material layer, absolutely
Edge material layer, the second metal material layer and the 3rd metal material layer composition, first metal material layer and insulation material layer are equal
The surface of polystyrene sphere is deposited on, and the first metal material layer and insulation material layer are docking together, second metal
Material layer depositions are in the upper surface of insulation material layer；3rd metal material layer is perpendicular to the second metal material layer and the first gold medal
Belong to material layer, and the 3rd metal material layer is deposited on the upper surface end of the first metal material layer and the second metal material layer；
The thickness of first metal material layer, the second metal material layer and the 3rd metal material layer is identical, and by identical
Metal deposit is formed；The thickness of the insulation material layer is more than first metal material layer, the second metal material layer and the 3rd
The thickness of metal material layer.
Preferably, the metal includes gold or silver, and the insulation material layer is silicon dioxide layer.
The preparation method of any of the above-described kind of tilted metallic nanostructured, comprises the following steps：
Step one：By polystyrene sphere model sheetinstallat in the substrate of glancing angle deposition plated film instrument, and it is evacuated to 3 × 10- 6Torr；
Step 2：It is 4 ° that polystyrene sphere stencil plane, which is adjusted, with vertical direction inclination angle, carries out the deposition of metal material, obtains
To the first metal material layer；
Step 3：After the completion of the deposition of step 2 metal material, rotation polystyrene sphere template makes 180 ° of its rotation, and protects
It is 4 ° that polystyrene sphere stencil plane, which is held, with vertical direction inclination angle, carries out the deposition of insulating materials, obtains insulation material layer；
Step 4：After step 3 obtains insulation material layer, keep the direction of polystyrene sphere template constant, gold is carried out again
Belong to the deposition of material, obtain the second metal material layer；
Step 5：After step 4 obtains the second metal material layer, keep consistent with direction of rotation in step 3 and rotate polyphenyl second
Alkene bead template, makes 90 ° of its rotation, and keeps polystyrene sphere stencil plane to be 4 ° with vertical direction inclination angle, carries out again
The deposition of metal material, obtains the 3rd metal material layer；
In above-mentioned steps, the sedimentation time all same of metal material, the sedimentation time of insulating materials is more than the deposition of metal material
Time.
Preferably, the sedimentation time of metal material is 300s, and the sedimentation time of insulating materials is 500 ~ 700s.
Preferably, when the direction of rotation in the step 3 and step 5 is clockwise, prepared structure is inclined to be left-handed
Oblique metal Nano structure；When the direction of rotation in the step 3 and step 5 is counterclockwise, prepared structure is inclined for dextrorotation
Oblique metal Nano structure.
Polystyrene sphere template in above-mentioned steps, its preparation method comprises the following steps：
Step 1, prepare plurality of glass sheets, and cleaned up；
Step 2, the sheet glass prepared in step 1 is laid in clean culture dish, deionized water is injected in culture, go from
Sub- water level will completely is not put into sheet glass therein, but to be less than the side wall top edge of culture dish；
Step 3, it is polystyrene sphere is ultrasonic three minutes, and polystyrene sphere mixed liquor is mixed into alcohol progress, will be poly-
Styrene bead mixed liquor inhalation syringe is with standby；
Step 4, culture dish side wall is close in the tangent plane side of the syringe needle of above-mentioned ready syringe, culture dish side must not be higher than
Wall edge, can not be contacted with horizontal plane, be slowly dropped into polystyrene sphere mixed liquor, make the polystyrene sphere slowly flowed down
Mixed liquor spreads in the water surface, forms the polystyrene sphere film of individual layer；
Step 5, with the polystyrene sphere film formed in Tx100 solution progressively polymerization procedure 4；
Step 6, the sheet glass being put into advance in step 2 is lifted with clean tweezers, polystyrene sphere monofilm will be attached with
Sheet glass be put into air-drying box, be adjusted to 40 DEG C and air-dried, obtain the polystyrene sphere template of individual layer.
Preferably, a diameter of 380 nm of the polystyrene sphere selected by the step 3, polystyrene sphere and alcohol
The mixed proportion of solution is 1：2~1：4.
Compared with prior art, beneficial effects of the present invention：
1. the structure of the present invention is deposited by template of polystyrene sphere, the gold of deposition is raised using deposition of insulative material
Belong to a part for material, make whole metal structure run-off the straight, and can be with by the sedimentation time for changing deposition of insulative material
Effectively change the inclined degree of metal structure, and its inclined degree is bigger, its circular dichroism is stronger；
2. and the tilted metallic nanostructured area that the method for the present invention is prepared is big, the optical detection after being easy to；
3. the method that the present invention prepares incline structure prepares incline structure compared to using technologies such as electron beam lithography and laser direct-writings
Method have step simple, save the time, and controllability it is strong the characteristics of；
4. the incline structure prepared using the method for the present invention is also applicable as strengthening the senser element of chiral molecules chiral information.
Brief description of the drawings
Fig. 1 is the deposition process schematic diagram of tilted metallic nanostructured of the present invention；
Fig. 2 is the right-handed spiral configuration schematic diagram of tilted metallic nanostructured of the present invention；
Fig. 3 is the left-handed spiral configuration schematic diagram of tilted metallic nanostructured of the present invention；
Fig. 4 is the SEM figures of tilted metallic nanometer left-handed spiral configuration prepared by the present invention；
Fig. 5 is the obtained circular dichroism of structure of sedimentation time difference of nonmetallic materials in the embodiment of the present invention 1,2,3
Figure；
In Fig. 1,1.：First metal material layer；②：Insulation material layer；③：Second metal material layer；④：3rd metal material
Layer；⑤：Polystyrene sphere；Arrow：Deposition direction.
Embodiment
Further detailed description is done to the present invention with reference to specific embodiment, but embodiments of the present invention are not limited to
This.
Embodiment 1：
Inclination as shown in Figure 2 is silver nanostructured, and the structure is deposited on the surface of polystyrene sphere, by the first silver layer, dioxy
SiClx layer, the second silver layer and the 3rd silver layer composition, the first silver layer and silicon dioxide layer are deposited on the surface of polystyrene sphere,
And first silver layer and silicon dioxide layer be docking together, the second silver layer is deposited on the upper surface of silicon dioxide layer；3rd silver layer hangs down
Directly in the second silver layer and the first silver layer, and the 3rd silver layer is deposited on the upper surface upper end of the first silver layer and the second silver layer；
The thickness of first silver layer, the second silver layer and the 3rd silver layer is identical, and the thickness of silicon dioxide layer is more than the first silver layer, the second silver medal
The thickness of layer and the 3rd silver layer.
Silver nanostructured deposition process is tilted as shown in figure 1, wherein 1. representing the first metal material layer, insulation is 2. represented
Material layer, 3. represents the second metal material layer, 4. represents the 3rd metal material layer, 5. represents polystyrene sphere, and arrow is represented
Deposition direction.
The present embodiment tilts silver nanostructured preparation method, comprises the following steps：
Step one：By polystyrene sphere model sheetinstallat in the substrate of glancing angle deposition plated film instrument, and it is evacuated to 3 × 10- 6Torr。
Step 2：It is 4 ° that polystyrene sphere stencil plane, which is adjusted, with vertical direction inclination angle, carries out the heavy of metal material
Product, sedimentation time is 300s, obtains the first metal material layer.
Step 3：After the completion of the deposition of step 2 metal material, the polystyrene sphere template that turns clockwise makes it certainly
Turn 180 °, and keep polystyrene sphere stencil plane to be 4 ° with vertical direction inclination angle, carry out the deposition of insulating materials, deposition
Time is 500s, obtains insulation material layer.
Step 4：After step 3 obtains insulation material layer, keep the direction of polystyrene sphere template constant, enter again
The deposition of row metal material, sedimentation time is 300s, obtains the second metal material layer.
Step 5：After step 4 obtains the second metal material layer, polystyrene sphere template clockwise makes its rotation
90 °, and keep polystyrene sphere stencil plane to be 4 ° with vertical direction inclination angle, the deposition of metal material, deposition are carried out again
Time is 300s, obtains the 3rd metal material layer.
Then cooling container, pours nitrogen, takes out sample.
In above-mentioned steps, the preparation method of polystyrene sphere template comprises the following steps：
Step 1, plurality of glass sheets is prepared, the width of sheet glass must not exceed 1 cm, and be cleaned up.
Step 2, the sheet glass prepared in step 1 is laid in clean culture dish, deionized water is injected in culture,
Deionized water liquid level will completely is not put into sheet glass therein, but will be less than culture dish side wall top edge, injection go from
Sub- water level is highly the 2/4-3/4 of culture dish height.
Step 3, it is polystyrene sphere is ultrasonic three minutes, and it is mixed into polystyrene sphere mixed liquor, polyphenyl with alcohol
The mixed proportion of a diameter of 380 nm of ethene bead, polystyrene sphere and alcoholic solution is 1:2-1:4；Polystyrene is small
Ball mixed liquor inhalation syringe is with standby.
Step 4, culture dish side wall is close in the tangent plane side of the syringe needle of above-mentioned ready syringe, must not be higher than culture
Ware side edge edge, can not be contacted with horizontal plane, be slowly dropped into polystyrene sphere mixed liquor, spread obtained individual layer polyphenyl second
Alkene bead film stops being added dropwise when being paved with the 3/5-4/5 of whole liquid level, and the polystyrene sphere mixed liquor slowly flowed down is in the water surface
Diffusion, forms the polystyrene sphere film of individual layer.
Step 5, with the polystyrene sphere film formed in Tx100 solution progressively polymerization procedure 4.
Step 6, the sheet glass being put into advance in step 2 is lifted with clean tweezers, polystyrene sphere list will be attached with
The sheet glass of tunic is put into air-drying box, is adjusted to 40 DEG C and is air-dried, and obtains the polystyrene sphere template of individual layer.
Manufactured in the present embodiment is tilted metallic nanometer right-handed spiral configuration.Its structure is as shown in Figure 2.
The structure of the present embodiment is put into cuvette, its circular dichroism is measured using normal incidence method in circular dichroism instrument
Signal, is obtained as the insulative material deposition time is 500s curve in Fig. 5.
The SEM of tilted metallic nanometer left-handed spiral configuration prepared by embodiment 1 is schemed as shown in figure 4, seeing from SEM image, the SEM
Figure is the right-handed spiral configuration into six close heap periodic structure arrangements shown in Fig. 2, from the figure, it can be seen that each periodic unit institute is right
A silver layer of correspondence first above the right-handed spiral configuration answered, its height is minimum, so color is most dark, a correspondence dioxy of lower section
SiClx insulate layer by layer with the second silver layer, one article of silver layer of correspondence the 3rd that left side is endways, consistent with the structure of the present invention.
Embodiment 2：
The preparation method of the present embodiment and the sedimentation time for differing only in silica of embodiment 1 are 600s, remaining with
Embodiment 1 is identical.
The obtained structure of the present embodiment is put into cuvette, it is measured using normal incidence method in circular dichroism instrument
Circular dichroism signal, obtains the curve for being 600s such as the sedimentation time of insulating materials in Fig. 5.
Embodiment 3：
The preparation method of the present embodiment and the sedimentation time for differing only in silica of embodiment 1 are 700s, remaining with
Embodiment 1 is identical.
The obtained structure of the present embodiment is put into cuvette, it is measured using normal incidence method in circular dichroism instrument
Circular dichroism signal, obtains the curve for being 700s such as the sedimentation time of insulating materials in Fig. 5.
Embodiment 4：
The preparation method of the present embodiment is that the metal material deposited is gold with the difference of embodiment 1, in step 3 and step 5
Middle rotation is to rotate counterclockwise, and remaining is same as Example 1.
What embodiment 4 was obtained is tilted metallic nanometer left-handed spiral configuration, as shown in figure 3, to be deposited on polystyrene small for the structure
The surface of ball, is made up of, the first layer gold and silicon dioxide layer are equal the first layer gold, silicon dioxide layer, the second layer gold and the 3rd layer gold
The surface of polystyrene sphere is deposited on, and the first layer gold and silicon dioxide layer are docking together, the second layer gold is deposited on dioxy
The upper surface of SiClx layer；3rd layer gold is perpendicular to the second layer gold and the first layer gold, and the 3rd layer gold is deposited on the first layer gold and
The upper surface bottom of two layer gold.
The structure of the present embodiment is put into cuvette, its circular dichroism signal is measured in circular dichroism instrument, can be seen
Arrive, tilted metallic nanostructured ratio does not have inclined metal Nano structure circular dichroism to be remarkably reinforced.
In addition, from Fig. 5 it can also be seen that the sedimentation time of insulating materials is longer, the circular dichroism of its structure is stronger, also
It is to say, the thickness of insulating materials is higher, and structure is more tilted, the circular dichroism of structure is stronger.
It should be noted that metal material is prepared in addition to Jin Yuyin using other metal materials in the structure of the present invention
The tilted metallic nanostructured gone out with gold it is identical with the tilted metallic nanostructured that silvery is standby, its circular dichroism also with Jin Yuyin
The tilted metallic nanostructured of preparation is similar, is that inclined degree is higher, its circular dichroism is stronger.
The structure of the present invention is deposited by template of polystyrene sphere, and deposition is raised using deposition of insulative material
A part for metal material, makes whole metal structure run-off the straight, and can by the sedimentation time for changing deposition of insulative material
Effectively to change the inclined degree of metal structure, and its inclined degree is bigger, and its circular dichroism is stronger；And the method for the present invention
The tilted metallic nanostructured area prepared is big, the optical detection after being easy to.
The method that the present invention prepares incline structure prepares bevelled junction compared to using technologies such as electron beam lithography and laser direct-writings
The method of structure has step simple, saves the time, and controllability it is strong the characteristics of, meanwhile, prepared using the method for the present invention
Incline structure is also applicable as strengthening the senser element of chiral molecules chiral information.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (7)
1. a kind of tilted metallic nanostructured, the structure is deposited on the surface of polystyrene sphere, it is characterised in that：By first
Metal material layer, insulation material layer, the second metal material layer and the 3rd metal material layer composition, first metal material layer and
Insulation material layer is deposited on the surface of polystyrene sphere, and the first metal material layer and insulation material layer are docking together,
Second metal material layer is deposited on the upper surface of insulation material layer；3rd metal material layer is perpendicular to the second metal material
The bed of material and the first metal material layer, and the 3rd metal material layer is deposited on the upper of the first metal material layer and the second metal material layer
Surface end；
The thickness of first metal material layer, the second metal material layer and the 3rd metal material layer is identical, and by identical
Metal deposit is formed；The thickness of the insulation material layer is more than first metal material layer, the second metal material layer and the 3rd
The thickness of metal material layer.
2. tilted metallic nanostructured according to claim 1, it is characterised in that：The metal includes gold or silver, described
Insulation material layer is silicon dioxide layer.
3. a kind of preparation method of tilted metallic nanostructured described in claim 1 or 2, it is characterised in that：Including following step
Suddenly：
Step one：By polystyrene sphere model sheetinstallat in the substrate of glancing angle deposition plated film instrument, and it is evacuated to 3 × 10- 6Torr；
Step 2：It is 4 ° that polystyrene sphere stencil plane, which is adjusted, with vertical direction inclination angle, carries out the deposition of metal material, obtains
To the first metal material layer；
Step 3：After step 2 obtains the first metal material layer, rotation polystyrene sphere template makes 180 ° of its rotation, and protects
It is 4 ° that polystyrene sphere stencil plane, which is held, with vertical direction inclination angle, carries out the deposition of insulating materials, obtains insulation material layer；
Step 4：After step 3 obtains insulation material layer, keep the direction of polystyrene sphere template constant, gold is carried out again
Belong to the deposition of material, obtain the second metal material layer；
Step 5：After step 4 obtains the second metal material layer, keep consistent with direction of rotation in step 3 and rotate polyphenyl second
Alkene bead template, makes 90 ° of its rotation, and keeps polystyrene sphere stencil plane to be 4 ° with vertical direction inclination angle, carries out again
The deposition of metal material, obtains the 3rd metal material layer；
In above-mentioned steps, the sedimentation time all same of metal material, the sedimentation time of insulating materials is more than the deposition of metal material
Time.
4. preparation method according to claim 3, it is characterised in that：The sedimentation time of metal material is 300s, insulation
The sedimentation time of material is 500 ~ 700s.
5. preparation method according to claim 3, it is characterised in that：Direction of rotation in the step 3 and step 5
For it is clockwise when, prepared structure is left-handed tilted metallic nanostructured；Rotation side in the step 3 and step 5
To for it is counterclockwise when, prepared structure is dextrorotation tilted metallic nanostructured.
6. preparation method according to claim 3, it is characterised in that：The polystyrene sphere template, its preparation method
Comprise the following steps：
Step 1, prepare plurality of glass sheets, and cleaned up；
Step 2, the sheet glass prepared in step 1 is laid in clean culture dish, deionized water is injected in culture dish, gone
Ion water level will completely is not put into sheet glass therein, but to be less than the side wall top edge of culture dish；
Step 3, it is polystyrene sphere is ultrasonic three minutes, and polystyrene sphere mixed liquor is mixed into alcohol, by polyphenyl second
Alkene bead mixed liquor inhalation syringe is with standby；
Step 4, culture dish side wall is close in the tangent plane side of the syringe needle of above-mentioned ready syringe, culture dish side must not be higher than
Wall edge, can not be contacted with horizontal plane, and polystyrene sphere mixed liquor is slowly dropped into culture dish, make the polyphenyl slowly flowed down
Ethene bead mixed liquor spreads in the water surface, forms the polystyrene sphere film of individual layer；
Step 5, with the polystyrene sphere film formed in Tx100 solution progressively polymerization procedure 4；
Step 6, the sheet glass being put into advance in step 2 is lifted with clean tweezers, polystyrene sphere monofilm will be attached with
Sheet glass be put into air-drying box, be adjusted to 40 DEG C and air-dried, obtain the polystyrene sphere template of individual layer.
7. preparation method according to claim 6, it is characterised in that：Polystyrene sphere selected by the step 3
The mixed proportion of a diameter of 380 nm, polystyrene sphere and alcoholic solution is 1：2~1：4.
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| CN109594047A (en) * | 2018-12-07 | 2019-04-09 | 中山科立特光电科技有限公司 | A kind of preparation method of chiral metal micro-nano helical structure |
| CN109709073A (en) * | 2019-01-10 | 2019-05-03 | 金华伏安光电科技有限公司 | A kind of nanometer of glomerular membrane number of plies detection device |
| CN109709073B (en) * | 2019-01-10 | 2021-10-22 | 苏州市东挺河智能科技发展有限公司 | Nano-microsphere film number detection device |
| CN110540170A (en) * | 2019-09-05 | 2019-12-06 | 陕西师范大学 | Metal micro-nano spiral structure and preparation method thereof |
| CN110668396A (en) * | 2019-09-16 | 2020-01-10 | 吉林师范大学 | Preparation method of periodic wavy nanopore structure array |
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