CN109913820A - A kind of preparation method of the three-dimensional chiral structure with difference in height - Google Patents
A kind of preparation method of the three-dimensional chiral structure with difference in height Download PDFInfo
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Abstract
The present invention relates to micro-nano structure preparation fields, and in particular to a kind of preparation method of the three-dimensional chiral structure with difference in height, comprising the following steps: Step 1: prepared by the template of chiral structure；Step 2: carrying out inclination plated film using the first deposition angles；Step 3: carrying out inclination plated film using the second deposition angles；Step 4: being handled, chiral structure is obtained；The preparation method of the three-dimensional chiral structure with difference in height, in preparation, there are when the chiral structure of difference in height, the processes such as carry out whirl coating repeatedly, electron beam exposure, alignment, development, fixing are not needed, only need to adjust the angle of deposit of plated film, the chiral structure there are difference in height can be prepared, so that preparing for the chiral structure with difference in height is more convenient, the requirement of electron beam lithography is reduced, the number of electron beam exposure is reduced.
Description
Technical field
The invention belongs to metal structure preparation fields, and in particular to a kind of preparation of the three-dimensional chiral structure with difference in height
Method.
Background technique
Chirality is used to indicate the symmetry of structure, there is important meaning in multiple subjects.Chirality refers to that object cannot be with
The property that its mirror image coincides, just as left hand and the right hand each other mirror image and can not be overlapped.Chirality is basic in life process
Feature, the exhausted big institute's number organic molecule for constituting life entity is all chiral molecules.
Researchers study the chiral mechanism generated and the senser element chiral as detection using artificial chiral structure,
Therefore, preparing chiral structure becomes extremely important.When preparation has the characteristics that the chiral structure of difference in height, need according to hand
Electron beam lithography is respectively adopted in the different height region of property structure, prepared by the mode of electron beam vacuum vapor plating, entirely
Preparation process needs carry out whirl coating repeatedly, electron beam exposure, alignment, development, fixing, plated film, removes photoresist, wherein alignment process ten
The cumbersome time-consuming divided, and it is easy to appear error, the failure of entire preparation structure may finally be caused.In addition to this, chiral knot
The different height of structure needs to be accurately positioned, and just can be carried out the preparation of next step, this for Nano grade chiral structure very
Difficulty, generally require to take a substantial amount of time.
Summary of the invention
In order to solve existing chiral structure preparation, there are complex procedures, preparation difficulty, time-consuming deficiency.
The preparation method of the present invention provides a kind of three-dimensional chiral structure with difference in height, comprising the following steps:
Step 1: prepared by the template of chiral structure；
Step 2: carrying out inclination plated film using the first deposition angles；
Step 3: carrying out inclination plated film using the second deposition angles；
Step 4: being handled, chiral structure is obtained.
It is described Step 1: specific steps prepared by the template of chiral structure are as follows:
(1) preparing substrate, and a layer photoresist is coated on substrate；
(2) design structure figure, and designed figure is formed with electron beam exposure corresponding region；
(3) substrate after overexposure is put into developer solution and is impregnated；
(4) by by drying after substrate be fixed, after dried with nitrogen, obtain the template of chiral structure.
The substrate is ito glass.
It is described Step 2: carrying out inclination plated film specific steps using the first deposition angles are as follows: will be prepared by step 1
The template of chiral structure is put into Electron beam evaporation instrument, is adjusted to the first deposition angles, carries out the vapor deposition of the first angle of deposit
Metal material.
Described rapid three, inclination plated film specific steps are carried out using the second deposition angles are as follows: by the deposition of the template of chiral structure
Angle is adjusted to the second deposition angles, carries out the evaporation metal material of the second angle of deposit.
It is described Step 4: handled, obtain chiral structure specific steps are as follows: the chiral knot of metal material will will be deposited
The template of structure, which is put into stripper, impregnates, and carries out lift-off stripping technology, after dried with nitrogen, and carry out SEM observation.
The angle of first deposition angles is greater than the angle of the second deposition angles.
The material of the plated film is gold, silver or copper.
Compared with prior art, beneficial effects of the present invention: the present invention provides this, and the three-dimensional with difference in height is chiral
The preparation method of structure, in preparation, there are the carry out whirl coating when chiral structure of difference in height, not needed repeatedly, electron beams to expose
The processes such as light, development, fixing eliminate all multi-steps being related to during alignment, and eliminate alignment and in the process may
Bring error.Only need to adjust the angle of deposit of plated film, so that it may which there are the chiral structures of difference in height for preparation, so that having height
It is more convenient to spend preparing for the chiral structure of difference, reduces the requirement of electron beam lithography, reduces time of electron beam exposure
Number.And there is no excessively high requirement to the width of electron beam exposure structure, but can equally be obtained finely by deposition angles deposition
Metal Nano structure.
Detailed description of the invention
Fig. 1 is that L shape chiral structure overlooks plated film schematic diagram.
Fig. 2 is L shape chiral structure side view plated film schematic diagram.
Fig. 3 is the circular dichroism figure of L shape chiral structure.
Fig. 4 is that F shape chiral structure overlooks plated film schematic diagram.
Fig. 5 is the circular dichroism figure of F shape chiral structure.
Specific embodiment
Embodiment 1
In order to solve existing chiral structure preparation there are complex procedures, preparation difficulty, time-consuming deficiency, the present invention is mentioned
Supply a kind of preparation method of three-dimensional chiral structure with difference in height, comprising the following steps:
Step 1: prepared by the template of chiral structure；
Step 2: carrying out inclination plated film using the first deposition angles；
Step 3: carrying out inclination plated film using the second deposition angles；
Step 4: being handled, chiral structure is obtained.
The preparation method of the three-dimensional chiral structure with difference in height, preparation there are the chiral structure of difference in height when
It waits, does not need the processes such as carry out whirl coating repeatedly, electron beam exposure, development, fixing, it is only necessary to the angle of deposit of plated film is adjusted,
The chiral structure there are difference in height can be prepared, so that preparing for the chiral structure with difference in height is more convenient, is reduced
The requirement of electron beam lithography reduces the number of electron beam exposure.
It is described Step 1: specific steps prepared by the template of chiral structure are as follows:
(1) preparing substrate, and a layer photoresist is coated on substrate；
(2) design structure figure, and designed figure is formed with electron beam exposure corresponding region；
(3) substrate after overexposure is put into developer solution and is impregnated；
(4) by by drying after substrate be fixed, after dried with nitrogen, obtain the template of chiral structure.
The substrate is ito glass.
It is described Step 2: carrying out inclination plated film specific steps using the first deposition angles are as follows: will be prepared by step 1
The template of chiral structure is put into Electron beam evaporation instrument, is adjusted to the first deposition angles, carries out the vapor deposition of the first angle of deposit
Metal material.
Described rapid three, inclination plated film specific steps are carried out using the second deposition angles are as follows: by the deposition of the template of chiral structure
Angle is adjusted to the second deposition angles, carries out the evaporation metal material of the second angle of deposit.
It is described Step 4: handled, obtain chiral structure specific steps are as follows: the chiral knot of metal material will will be deposited
The template of structure, which is put into stripper, impregnates, and carries out lift-off stripping technology, after dried with nitrogen, and carry out SEM observation.
The material of the plated film is gold, silver or copper.
Embodiment 2
A kind of preparation method of the three-dimensional chiral structure with difference in height, the preparation method of chiral structure, including following step
It is rapid:
Step 1: prepared by the template of chiral structure, specific steps are as follows:
(1) prepare ito glass, ito glass, will be quasi- having a size of 20.0mm × 10.0mm with a thickness of 1.0mm, length x width
Standby ito glass, which is put into cleaning solution, to be cleaned, super with acetone ultrasound 15min, then with alcohol after deionized water ultrasound 15min
Sound 15min uses deionized water ultrasound 5min later, is put into after finally being dried up with nitrogen gun spare in nitrogen cabinet；In use, serving as a contrast
A layer photoresist is coated on bottom；Specifically, the photoresist is polymethyl methacrylate (PMMA), and coating photoresist is with getting rid of
Glue machine coats in ready glass substrate, and the revolving speed of the photoresist spinner is 6000rpm, time 60s.Coat photoresist
With a thickness of 30~50nm.The temperature of drying is 150 DEG C, time 3min.
(2) design structure figure, and designed figure is formed with electron beam exposure corresponding region；Designed figure must
It must meet on a certain determining direction that there are width is poor, i.e., as shown in Figure 1, institute's plated film width is when chiral structure width is m
When l, there are a region (m-l) non-plated films；The a certain determining direction, with projecting direction phase of the vapor deposition direction on stencil plane
Together.
(3) substrate after overexposure is put into developer solution and is impregnated, carry out development operation, the time for impregnating development is
30s~80s；Common developer solution can be made of isopropanol, methanol and deionized water；
(4) by by drying after substrate be fixed, after dried with nitrogen, obtain the template of chiral structure；It is common
Fixing solution is made of main components such as fixer, hardener, protective agent acid.
Step 2: carrying out the specific steps of inclination plated film using the first deposition angles are as follows: the hand that will be prepared by step 1
Property structure template be put into Electron beam evaporation instrument, be adjusted to the first deposition angles, carry out the vapor deposition gold of the first angle of deposit
Belong to material.
Step 3: carrying out the specific steps of inclination plated film using the second deposition angles are as follows: by the deposition of the template of chiral structure
Angle is adjusted to the second deposition angles, carries out the evaporation metal material of the second angle of deposit.
The angle of first deposition angles is greater than the angle of the second deposition angles, in this way, carrying out the angle of a deposition angles
When plated film, chiral structure integrally can be carried out plated film, can only give chiral structure in the angle for carrying out the second deposition angles
Part carries out plated film, and material is thus formed differences in height, to prepare satisfactory chiral structure.The angle of first deposition angles
It is expressed asThe angle of second deposition angles is expressed asWherein, h is the thickness of whirl coating, and m is structure chart
The width of shape；L is the width that plated film forms the lower metal structure of thickness.
The evaporation metal material of first angle of deposit, the evaporation metal material of the second angle of deposit can use electron beam
Vacuum evaporating coating machine carries out plated film, and the vacuum degree of electron beam vacuum evaporating coating machine is not more than 3 × 10-6Torr, evaporation metal
The rate of material isThe material of plated film can be gold, silver or copper.
Step 4: being handled, the specific steps of chiral structure are obtained are as follows: the chiral structure of metal material will will be deposited
Template be put into stripper and impregnate, carry out lift-off stripping technology, after dried with nitrogen, and carry out SEM observation.
Embodiment 3
Using a kind of preparation method of above-mentioned three-dimensional chiral structure with difference in height, L shape hand as shown in Figure 1 is prepared
Property structure, comprising the following steps:
Step 1: prepared by the template of chiral structure, specific steps are as follows:
(1) prepare ito glass, ito glass, will be quasi- having a size of 20.0mm × 10.0mm with a thickness of 1.0mm, length x width
Standby ito glass, which is put into cleaning solution, to be cleaned, super with acetone ultrasound 15min, then with alcohol after deionized water ultrasound 15min
Sound 15min uses deionized water ultrasound 5min later, is put into after finally being dried up with nitrogen gun spare in nitrogen cabinet；In use, passing through
Photoresist spinner coats one layer of PMMA photoresist on substrate, and the revolving speed of the photoresist spinner is 6000rpm, time 60s.Coat photoetching
Glue with a thickness of 50nm, the temperature of drying is 150 DEG C, time 3min.
(2) design structure figure is L shape, and designed L figure is formed with electron beam exposure corresponding region；
(3) substrate after overexposure is put into developer solution and is impregnated, carry out development operation, the time for impregnating development is
60s；Common developer solution can be made of isopropanol, methanol and deionized water；
(4) by by drying after substrate be fixed, after dried with nitrogen, obtain the template of chiral structure；It is common
Fixing solution is made of main components such as fixer, hardener, protective agent acid.
Step 2: carrying out the specific steps of inclination plated film using the first deposition angles are as follows: the hand that will be prepared by step 1
Property structure template be put into Electron beam evaporation instrument, be adjusted to the first deposition angles, carry out the vapor deposition gold of the first angle of deposit
Belong to material.
Step 3: carrying out the specific steps of inclination plated film using the second deposition angles are as follows: by the deposition of the template of chiral structure
Angle is adjusted to the second deposition angles, carries out the evaporation metal material of the second angle of deposit.
It should be noted that inclined angle must select the right side of L-shaped structure, right side protrusion just can use in this way
Fill part adjusts coating film thickness, as shown in Figure 2.
The angle of first deposition angles is greater than the angle of the second deposition angles, in this way, carrying out the angle of a deposition angles
When plated film, plated film can integrally can be carried out to L shape chiral structure, can only give L in the angle for carrying out the second deposition angles
The transverse arm of shape chiral structure carries out plated film, and arm vertical in this way and transverse arm will form difference in height, meet to prepare
It is required that L shape chiral structure.The angle of first deposition angles is expressed asThe angle of second deposition angles is expressed asWherein, h is the thickness of whirl coating, and m is the width of structure graph；L is that plated film forms the lower metal structure of thickness
Width.
The evaporation metal material of first angle of deposit, the evaporation metal material of the second angle of deposit can use electron beam
Vacuum evaporating coating machine carries out plated film, and the vacuum degree of electron beam vacuum evaporating coating machine is not more than 3*10-6torr, evaporation metal
The rate of material isThe material of plated film can be gold, silver or copper.
Step 4: being handled, the specific steps of chiral structure are obtained are as follows: the chiral structure of metal material will will be deposited
Template be put into stripper and impregnate, carry out lift-off stripping technology, after dried with nitrogen, and carry out SEM observation.
It is illustrated in figure 3 prepared by the preparation method according to the three-dimensional chiral structure shown in the present embodiment with difference in height
L shape chiral structure circular dichroism figure, the size of L shape chiral structure are as follows: the length x width x thickness of vertical arm
For 600.0mm × 90.0mm × 90.0mm, the length x width x thickness of transverse arm be 450.0mm × 90.0mm ×
180.0mm, it can be seen that having apparent circular dichroism signal when a length of 680nm of light wave.
Embodiment 4
Using a kind of preparation method of above-mentioned three-dimensional chiral structure with difference in height, F shape hand as shown in Figure 4 is prepared
Property structure, comprising the following steps:
Step 1: prepared by the template of chiral structure, specific steps are as follows:
(1) prepare ito glass, ito glass, will be quasi- having a size of 20.0mm × 10.0mm with a thickness of 1.0mm, length x width
Standby ito glass, which is put into cleaning solution, to be cleaned, super with acetone ultrasound 15min, then with alcohol after deionized water ultrasound 15min
Sound 15min uses deionized water ultrasound 5min later, is put into after finally being dried up with nitrogen gun spare in nitrogen cabinet；In use, passing through
Photoresist spinner coats one layer of PMMA photoresist on substrate, and the revolving speed of the photoresist spinner is 6000rpm, time 60s.Coat photoetching
Glue with a thickness of 50nm, the temperature of drying is 150 DEG C, time 3min.
(2) design structure figure is F shape, and designed F figure is formed with electron beam exposure corresponding region；
(3) substrate after overexposure is put into developer solution and is impregnated, carry out development operation, the time for impregnating development is
60s；Common developer solution can be made of isopropanol, methanol and deionized water；
(4) by by drying after substrate be fixed, after dried with nitrogen, obtain the template of chiral structure；It is common
Fixing solution is made of main components such as fixer, hardener, protective agent acid.
Step 2: carrying out the specific steps of inclination plated film using the first deposition angles are as follows: the hand that will be prepared by step 1
Property structure template be put into Electron beam evaporation instrument, be adjusted to the first deposition angles, carry out the vapor deposition gold of the first angle of deposit
Belong to material.
Step 3: carrying out the specific steps of inclination plated film using the second deposition angles are as follows: by the deposition of the template of chiral structure
Angle is adjusted to the second deposition angles, carries out the evaporation metal material of the second angle of deposit.
It should be noted that inclined angle must select the right side of F shape structure, right side protrusion just can use in this way
Fill part adjusts coating film thickness, as shown in Figure 4.
The angle of first deposition angles is greater than the angle of the second deposition angles, in this way, carrying out the angle of a deposition angles
When plated film, plated film can integrally can be carried out to F shape chiral structure, can only give F in the angle for carrying out the second deposition angles
The first transverse arm, the second transverse arm of shape chiral structure carry out plated film, and arm vertical in this way and the first transverse arm, the second transverse arm are just
Difference in height is will form, to prepare satisfactory F shape chiral structure.The angle of first deposition angles is expressed asThe angle of second deposition angles is expressed asWherein, h is the thickness of whirl coating, and m is the width of structure graph
Degree；L is the width that plated film forms the lower metal structure of thickness.
The evaporation metal material of first angle of deposit, the evaporation metal material of the second angle of deposit can use electron beam
Vacuum evaporating coating machine carries out plated film, and the vacuum degree of electron beam vacuum evaporating coating machine is not more than 3 × 10-6Torr, evaporation metal
The rate of material isThe material of plated film can be gold, silver or copper.
Step 4: being handled, the specific steps of chiral structure are obtained are as follows: the chiral structure of metal material will will be deposited
Template be put into stripper and impregnate, carry out lift-off stripping technology, after dried with nitrogen, and carry out SEM observation.
It is illustrated in figure 5 prepared by the preparation method according to the three-dimensional chiral structure shown in the present embodiment with difference in height
F shape chiral structure circular dichroism figure, the size of F shape chiral structure are as follows: the length x width x thickness of vertical arm
For 600.0mm × 90.0mm × 90.0mm, the length x width x thickness of the first transverse arm be 450.0mm × 90.0mm ×
180.0mm, the length x width x thickness of the second transverse arm are 450.0mm × 150.0mm × 180.0mm, can from figure
See, as light wave a length of 950nm, 1390nm, there is apparent circular dichroism signal.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (8)
1. a kind of preparation method of the three-dimensional chiral structure with difference in height, which comprises the following steps:
Step 1: prepared by the template of chiral structure；
Step 2: carrying out inclination plated film using the first deposition angles；
Step 3: carrying out inclination plated film using the second deposition angles；
Step 4: being handled, chiral structure is obtained.
2. a kind of preparation method of the three-dimensional chiral structure with difference in height as described in claim 1, which is characterized in that described
Step 1: specific steps prepared by the template of chiral structure are as follows:
(1) preparing substrate, and a layer photoresist is coated on substrate；
(2) design structure figure, and designed figure is formed with electron beam exposure corresponding region；
(3) substrate after overexposure is put into developer solution and is impregnated；
(4) by by drying after substrate be fixed, after dried with nitrogen, obtain the template of chiral structure.
3. a kind of preparation method of three-dimensional chiral structure with difference in height according to claim 2, it is characterised in that: institute
Stating substrate is ito glass.
4. a kind of preparation method of the three-dimensional chiral structure with difference in height as described in claim 1, which is characterized in that described
Step 2: carrying out inclination plated film specific steps using the first deposition angles are as follows: by the mould of the chiral structure prepared by step 1
Plate is put into Electron beam evaporation instrument, is adjusted to the first deposition angles, carries out the evaporation metal material of the first angle of deposit.
5. a kind of preparation method of the three-dimensional chiral structure with difference in height as described in claim 1, which is characterized in that described
Rapid three, inclination plated film specific steps are carried out using the second deposition angles are as follows: the angle of deposit of the template of chiral structure is adjusted to the
Two deposition angles carry out the evaporation metal material of the second angle of deposit.
6. a kind of preparation method of the three-dimensional chiral structure with difference in height as described in claim 1, which is characterized in that described
Step 4: being handled, chiral structure specific steps are obtained are as follows: the template that the chiral structure of metal material has been deposited will be put into
Impregnated in stripper, carry out lift-off stripping technology, after dried with nitrogen, and carry out SEM observation.
7. a kind of preparation method of the three-dimensional chiral structure with difference in height as described in claim 1, it is characterised in that: described
The angle of first deposition angles is greater than the angle of the second deposition angles.
8. a kind of preparation method of the three-dimensional chiral structure with difference in height as described in claim 1, it is characterised in that: described
The material of plated film is gold, silver or copper.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110160997A (en) * | 2019-07-02 | 2019-08-23 | 陕西师范大学 | A kind of waveguiding structure for realizing chiral near field and its chiral detection method |
| CN110515280A (en) * | 2019-09-05 | 2019-11-29 | 陕西师范大学 | A method of preparing the chiral micro-nano structure of thin space |
| CN110531446A (en) * | 2019-09-05 | 2019-12-03 | 陕西师范大学 | A kind of U-shaped structure and preparation method thereof for realizing circular dichroism |
| CN111188011A (en) * | 2020-02-17 | 2020-05-22 | 陕西师范大学 | Three-dimensional chiral conical metal nanoshell with height difference and preparation method thereof |
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| CN106395738A (en) * | 2016-11-10 | 2017-02-15 | 陕西师范大学 | Chiral nanostructure with adjustable circular dichroism and preparation method thereof |
| CN107144909A (en) * | 2017-04-06 | 2017-09-08 | 陕西师范大学 | It is a kind of to realize single layer of gold nanostructured of asymmetric transmission and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106395738A (en) * | 2016-11-10 | 2017-02-15 | 陕西师范大学 | Chiral nanostructure with adjustable circular dichroism and preparation method thereof |
| CN107144909A (en) * | 2017-04-06 | 2017-09-08 | 陕西师范大学 | It is a kind of to realize single layer of gold nanostructured of asymmetric transmission and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110160997A (en) * | 2019-07-02 | 2019-08-23 | 陕西师范大学 | A kind of waveguiding structure for realizing chiral near field and its chiral detection method |
| CN110160997B (en) * | 2019-07-02 | 2021-07-06 | 陕西师范大学 | Waveguide structure for realizing chiral near field and chiral detection method thereof |
| CN110515280A (en) * | 2019-09-05 | 2019-11-29 | 陕西师范大学 | A method of preparing the chiral micro-nano structure of thin space |
| CN110531446A (en) * | 2019-09-05 | 2019-12-03 | 陕西师范大学 | A kind of U-shaped structure and preparation method thereof for realizing circular dichroism |
| CN110515280B (en) * | 2019-09-05 | 2021-08-13 | 陕西师范大学 | Method for preparing narrow-spacing chiral micro-nano structure |
| CN111188011A (en) * | 2020-02-17 | 2020-05-22 | 陕西师范大学 | Three-dimensional chiral conical metal nanoshell with height difference and preparation method thereof |
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