CN109913820B - Preparation method of three-dimensional chiral structure with height difference - Google Patents
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Abstract
The invention relates to the field of micro-nano structure preparation, in particular to a preparation method of a three-dimensional chiral structure with height difference, which comprises the following steps: step one, preparing a template with a chiral structure; step two, performing inclined film coating by adopting a first deposition angle; step three, performing inclined film coating by adopting a second deposition angle; step four, processing to obtain a chiral structure; according to the preparation method of the three-dimensional chiral structure with the height difference, when the chiral structure with the height difference is prepared, the chiral structure with the height difference can be prepared only by adjusting the deposition angle of a coating film without repeatedly performing the processes of whirl coating, electron beam exposure, alignment, development, fixation and the like, so that the preparation of the chiral structure with the height difference is more convenient, the requirements of an electron beam exposure technology are reduced, and the times of electron beam exposure are reduced.
Description
Technical Field
The invention belongs to the field of metal structure preparation, and particularly relates to a preparation method of a three-dimensional chiral structure with a height difference.
Background
Chirality is used to indicate structural symmetry and is of great significance in a number of disciplines. Chirality refers to the property of an object not coinciding with its mirror image, as if the left and right hands were mirror images of each other. Chirality is a fundamental feature in the life process, and most of the organic molecules that make up a living body are chiral molecules.
Researchers have utilized artificial chiral structures to study the mechanism of chiral generation and as sensing devices for detecting chirality, and thus, the preparation of chiral structures has become very important. When a chiral structure with the height difference characteristic is prepared, electron beam etching and electron beam vacuum evaporation coating methods are required to be respectively adopted according to different height areas of the chiral structure for preparation, the whole preparation process needs repeated photoresist throwing, electron beam exposure, alignment, development, fixation, coating and photoresist removing, the alignment process is very complicated and time-consuming, errors are easy to occur, and finally the whole preparation structure can fail. In addition, different heights of the chiral structure need to be accurately positioned for the next step of preparation, which is very difficult for the chiral structure at the nanometer level and often needs a lot of time.
Disclosure of Invention
The method aims to solve the defects of complex process, difficult preparation and time consumption in the existing chiral structure preparation.
The invention provides a preparation method of a three-dimensional chiral structure with height difference, which comprises the following steps:
step one, preparing a template with a chiral structure;
step two, performing inclined film coating by adopting a first deposition angle;
step three, performing inclined film coating by adopting a second deposition angle;
and step four, processing to obtain the chiral structure.
The first step, the preparation of the template with the chiral structure comprises the following specific steps:
(1) preparing a substrate, and coating a layer of photoresist on the substrate;
(2) designing a structural pattern, and exposing a corresponding area by using an electron beam to form the designed pattern;
(3) soaking the exposed substrate in a developing solution;
(4) and (3) fixing the dried substrate, and drying by using nitrogen to obtain the template with the chiral structure.
The substrate is ITO glass.
The second step of performing inclined film coating by adopting the first deposition angle comprises the following specific steps: and (4) placing the template with the chiral structure prepared in the first step into an electron beam vacuum coating instrument, adjusting the template to a first deposition angle, and performing metal material evaporation at the first deposition angle.
The third step of performing inclined film coating by adopting a second deposition angle comprises the following specific steps: and adjusting the deposition angle of the template with the chiral structure to be a second deposition angle, and performing metal evaporation at the second deposition angle.
The fourth step of processing to obtain the chiral structure comprises the following specific steps: and (3) putting the template with the chiral structure of the metal material after evaporation into stripping liquid for soaking, performing lift-off stripping process, drying by using nitrogen, and performing SEM observation.
The angle of the first deposition angle is greater than the angle of the second deposition angle.
The coating film is made of gold, silver or copper.
Compared with the prior art, the invention has the beneficial effects that: the invention provides the preparation method of the three-dimensional chiral structure with the height difference, when the chiral structure with the height difference is prepared, the repeated working procedures of whirl coating, electron beam exposure, development, fixation and the like are not needed, a plurality of steps involved in the alignment process are omitted, and errors possibly brought in the alignment process are eliminated. The chiral structure with the height difference can be prepared only by adjusting the deposition angle of the coating film, so that the preparation of the chiral structure with the height difference is more convenient, the requirements of an electron beam exposure technology are reduced, and the times of electron beam exposure are reduced. And there is no excessive requirement for the width of the electron beam exposed structure, but fine metal nanostructures can be obtained by deposition at the deposition angle as well.
Drawings
FIG. 1 is a schematic view of a L-shaped chiral structure of a top-down coating film.
FIG. 2 is a schematic diagram of a side-view coating of an L-shaped chiral structure.
FIG. 3 is a circular dichroism spectrum of an L-shaped chiral structure.
FIG. 4 is a schematic view of a top-down coating of an F-shaped chiral structure.
FIG. 5 is a circular dichroism spectrum of an F-shaped chiral structure.
Detailed Description
Example 1
In order to solve the defects of complex process, difficult preparation and time consumption in the existing chiral structure preparation, the invention provides a preparation method of a three-dimensional chiral structure with a height difference, which comprises the following steps:
step one, preparing a template with a chiral structure;
step two, performing inclined film coating by adopting a first deposition angle;
step three, performing inclined film coating by adopting a second deposition angle;
and step four, processing to obtain the chiral structure.
According to the preparation method of the three-dimensional chiral structure with the height difference, when the chiral structure with the height difference is prepared, the chiral structure with the height difference can be prepared only by adjusting the deposition angle of a coating film without repeatedly performing the processes of whirl coating, electron beam exposure, development, fixation and the like, so that the preparation of the chiral structure with the height difference is more convenient, the requirements of an electron beam exposure technology are reduced, and the times of electron beam exposure are reduced.
The first step, the preparation of the template with the chiral structure comprises the following specific steps:
(1) preparing a substrate, and coating a layer of photoresist on the substrate;
(2) designing a structural pattern, and exposing a corresponding area by using an electron beam to form the designed pattern;
(3) soaking the exposed substrate in a developing solution;
(4) and (3) fixing the dried substrate, and drying by using nitrogen to obtain the template with the chiral structure.
The substrate is ITO glass.
The second step of performing inclined film coating by adopting the first deposition angle comprises the following specific steps: and (4) placing the template with the chiral structure prepared in the first step into an electron beam vacuum coating instrument, adjusting the template to a first deposition angle, and performing metal material evaporation at the first deposition angle.
The third step of performing inclined film coating by adopting a second deposition angle comprises the following specific steps: and adjusting the deposition angle of the template with the chiral structure to be a second deposition angle, and performing metal evaporation at the second deposition angle.
The fourth step of processing to obtain the chiral structure comprises the following specific steps: and (3) putting the template with the chiral structure of the metal material after evaporation into stripping liquid for soaking, performing lift-off stripping process, drying by using nitrogen, and performing SEM observation.
The coating film is made of gold, silver or copper.
Example 2
A method for preparing a three-dimensional chiral structure with a height difference comprises the following steps:
step one, preparing a template with a chiral structure, which comprises the following specific steps:
(1) preparing ITO glass, wherein the thickness of the ITO glass is 1.0mm, the length multiplied by the width dimension is 20.0mm multiplied by 10.0mm, the prepared ITO glass is put into a washing solution for washing, is subjected to ultrasonic treatment by deionized water for 15min, is subjected to ultrasonic treatment by acetone for 15min, is subjected to ultrasonic treatment by alcohol for 15min, is subjected to ultrasonic treatment by deionized water for 5min, and is finally dried by a nitrogen gun and then is put into a nitrogen cabinet for standby; when in use, a layer of photoresist is coated on the substrate; specifically, the photoresist is polymethyl methacrylate (PMMA), the photoresist is coated on the prepared glass substrate by using a spin coater, the rotating speed of the spin coater is 6000rpm, and the time is 60 s. The thickness of the coating photoresist is 30-50 nm. The drying temperature is 150 deg.C, and the drying time is 3 min.
(2) Designing a structural pattern, and exposing a corresponding area by using an electron beam to form the designed pattern; the designed pattern has to satisfy the width difference in a certain direction, that is, as shown in fig. 1, when the width of the chiral structure is m, and the width of the coated film is l, an area (m-l) is not coated; and the certain determined direction is the same as the projection direction of the evaporation direction on the template plane.
(3) Soaking the exposed substrate in a developing solution for development for 30-80 s; a typical developer solution may consist of isopropanol, methanol, and deionized water;
(4) fixing the dried substrate, and drying with nitrogen to obtain a template with a chiral structure; a general fixer fluid is composed of main components such as a fixer, a film hardener, and a protective agent acid.
Step two, the specific steps of adopting the first deposition angle to carry out inclined film coating are as follows: and (4) placing the template with the chiral structure prepared in the first step into an electron beam vacuum coating instrument, adjusting the template to a first deposition angle, and performing metal material evaporation at the first deposition angle.
Step three, the specific steps of performing inclined film coating by adopting a second deposition angle are as follows: and adjusting the deposition angle of the template with the chiral structure to be a second deposition angle, and performing metal evaporation at the second deposition angle.
The angle of the first deposition angle is larger than that of the second deposition angle, so that the whole chiral structure can be coated when the coating at the angle of the first deposition angle is carried out, and only the part of the chiral structure can be coated when the coating at the angle of the second deposition angle is carried out, so that the height difference is formed, and the chiral structure meeting the requirements is prepared. The angle of the first deposition angle is expressed as
The angle of the second deposition angle is expressed as
Wherein h is the thickness of the spin coating, and m is the width of the structural pattern; l is the width of the metal structure with lower thickness formed by the plated film.
The evaporated metal material at the first deposition angle and the evaporated metal material at the second deposition angle can be coated by an electron beam vacuum evaporation coating machine, and the vacuum degree of the electron beam vacuum evaporation coating machine is not more than 3 multiplied by 10-6torr, rate of evaporating metal material
The material of the coating film can be gold, silver or copper.
Step four, processing to obtain a chiral structure, which comprises the following specific steps: and (3) putting the template with the chiral structure of the metal material after evaporation into stripping liquid for soaking, performing lift-off stripping process, drying by using nitrogen, and performing SEM observation.
Example 3
The method for preparing the three-dimensional chiral structure with the height difference is used for preparing the L-shaped chiral structure shown in the figure 1, and comprises the following steps:
step one, preparing a template with a chiral structure, which comprises the following specific steps:
(1) preparing ITO glass, wherein the thickness of the ITO glass is 1.0mm, the length multiplied by the width dimension is 20.0mm multiplied by 10.0mm, the prepared ITO glass is put into a washing solution for washing, is subjected to ultrasonic treatment by deionized water for 15min, is subjected to ultrasonic treatment by acetone for 15min, is subjected to ultrasonic treatment by alcohol for 15min, is subjected to ultrasonic treatment by deionized water for 5min, and is finally dried by a nitrogen gun and then is put into a nitrogen cabinet for standby; when the PMMA photoresist is used, a layer of PMMA photoresist is coated on a substrate through a photoresist spinner, the rotating speed of the photoresist spinner is 6000rpm, and the time is 60 s. The thickness of the coated photoresist is 50nm, the drying temperature is 150 ℃, and the time is 3 min.
(2) Designing the structural pattern to be L-shaped, and exposing the corresponding area by using an electron beam to form a designed L-shaped pattern;
(3) soaking the exposed substrate in a developing solution for development for 60 s; a typical developer solution may consist of isopropanol, methanol, and deionized water;
(4) fixing the dried substrate, and drying with nitrogen to obtain a template with a chiral structure; a general fixer fluid is composed of main components such as a fixer, a film hardener, and a protective agent acid.
Step two, the specific steps of adopting the first deposition angle to carry out inclined film coating are as follows: and (4) placing the template with the chiral structure prepared in the first step into an electron beam vacuum coating instrument, adjusting the template to a first deposition angle, and performing metal material evaporation at the first deposition angle.
Step three, the specific steps of performing inclined film coating by adopting a second deposition angle are as follows: and adjusting the deposition angle of the template with the chiral structure to be a second deposition angle, and performing metal evaporation at the second deposition angle.
It should be noted that the inclined angle must be selected on the right side of the L-shaped structure, so that the thickness of the plated film can be adjusted by using the filling portion of the right protrusion, as shown in fig. 2.
The angle of the first deposition angle is larger than that of the second deposition angle, so that when coating at the angle of the first deposition angle is carried out, coating can be carried out at the angle of the second deposition angleThe L-shaped chiral structure can be coated integrally, and the transverse arm of the L-shaped chiral structure can be coated at the angle of the second deposition angle, so that the vertical arm and the transverse arm can form a height difference, and the L-shaped chiral structure meeting the requirement is prepared. The angle of the first deposition angle is expressed as
The angle of the second deposition angle is expressed as
Wherein h is the thickness of the spin coating, and m is the width of the structural pattern; l is the width of the metal structure with lower thickness formed by the plated film.
The evaporated metal material at the first deposition angle and the evaporated metal material at the second deposition angle can be coated by an electron beam vacuum evaporation coating machine, the vacuum degree of the electron beam vacuum evaporation coating machine is not more than 3 x 10-6torr, and the speed of the evaporated metal material is
The material of the coating film can be gold, silver or copper.
Step four, processing to obtain a chiral structure, which comprises the following specific steps: and (3) putting the template with the chiral structure of the metal material after evaporation into stripping liquid for soaking, performing lift-off stripping process, drying by using nitrogen, and performing SEM observation.
As shown in fig. 3, a circular dichroism spectrum of an L-shaped chiral structure prepared according to the method for preparing a three-dimensional chiral structure having a height difference shown in this example is shown, and the size of the L-shaped chiral structure is: the vertical arms have length x width x thickness dimensions of 600.0mm x 90.0mm and the transverse arms have length x width x thickness dimensions of 450.0mm x 90.0mm x 180.0mm, it being seen that a circular dichroism signal is evident at a light wavelength of 680 nm.
Example 4
The method for preparing the three-dimensional chiral structure with the height difference is used for preparing the F-shaped chiral structure shown in the figure 4, and comprises the following steps:
step one, preparing a template with a chiral structure, which comprises the following specific steps:
(1) preparing ITO glass, wherein the thickness of the ITO glass is 1.0mm, the length multiplied by the width dimension is 20.0mm multiplied by 10.0mm, the prepared ITO glass is put into a washing solution for washing, is subjected to ultrasonic treatment by deionized water for 15min, is subjected to ultrasonic treatment by acetone for 15min, is subjected to ultrasonic treatment by alcohol for 15min, is subjected to ultrasonic treatment by deionized water for 5min, and is finally dried by a nitrogen gun and then is put into a nitrogen cabinet for standby; when the PMMA photoresist is used, a layer of PMMA photoresist is coated on a substrate through a photoresist spinner, the rotating speed of the photoresist spinner is 6000rpm, and the time is 60 s. The thickness of the coated photoresist is 50nm, the drying temperature is 150 ℃, and the time is 3 min.
(2) Designing the structural pattern to be F-shaped, and exposing a corresponding area by using an electron beam to form a designed F-shaped pattern;
(3) soaking the exposed substrate in a developing solution for development for 60 s; a typical developer solution may consist of isopropanol, methanol, and deionized water;
(4) fixing the dried substrate, and drying with nitrogen to obtain a template with a chiral structure; a general fixer fluid is composed of main components such as a fixer, a film hardener, and a protective agent acid.
Step two, the specific steps of adopting the first deposition angle to carry out inclined film coating are as follows: and (4) placing the template with the chiral structure prepared in the first step into an electron beam vacuum coating instrument, adjusting the template to a first deposition angle, and performing metal material evaporation at the first deposition angle.
Step three, the specific steps of performing inclined film coating by adopting a second deposition angle are as follows: and adjusting the deposition angle of the template with the chiral structure to be a second deposition angle, and performing metal evaporation at the second deposition angle.
It should be noted that the angle of inclination must be selected to the right side of the F-shaped structure, so that the thickness of the plated film can be adjusted by using the filling portion of the right side protrusion, as shown in fig. 4.
The angle of the first deposition angle is larger than that of the second deposition angle, so that the whole F-shaped chiral structure can be coated when the coating at the angle of the first deposition angle is carried outAnd (3) coating, namely coating films on the first transverse arm and the second transverse arm of the F-shaped chiral structure at the angle of the second deposition angle, so that the vertical arm, the first transverse arm and the second transverse arm form a height difference, and the F-shaped chiral structure meeting the requirement is prepared. The angle of the first deposition angle is expressed as
The angle of the second deposition angle is expressed as
Wherein h is the thickness of the spin coating, and m is the width of the structural pattern; l is the width of the metal structure with lower thickness formed by the plated film.
The evaporated metal material at the first deposition angle and the evaporated metal material at the second deposition angle can be coated by an electron beam vacuum evaporation coating machine, and the vacuum degree of the electron beam vacuum evaporation coating machine is not more than 3 multiplied by 10-6torr, rate of evaporating metal material
The material of the coating film can be gold, silver or copper.
Step four, processing to obtain a chiral structure, which comprises the following specific steps: and (3) putting the template with the chiral structure of the metal material after evaporation into stripping liquid for soaking, performing lift-off stripping process, drying by using nitrogen, and performing SEM observation.
As shown in fig. 5, a circular dichroism spectrum of the F-shaped chiral structure prepared according to the method for preparing the three-dimensional chiral structure having the height difference shown in this example is shown, and the dimensions of the F-shaped chiral structure are: the vertical arm has length × width × thickness dimensions of 600.0mm × 90.0mm × 90.0mm, the first lateral arm has length × width × thickness dimensions of 450.0mm × 90.0mm × 180.0mm, and the second lateral arm has length × width × thickness dimensions of 450.0mm × 150.0mm × 180.0mm, and as can be seen from the figure, when the light wavelengths are 950nm and 1390nm, a circular dichroism signal is evident.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (5)
1. A method for preparing a three-dimensional chiral structure with a height difference is characterized by comprising the following steps:
step one, preparing a template with a chiral structure;
step two, performing inclined film coating by adopting a first deposition angle; the second step specifically comprises: putting the template with the chiral structure prepared in the first step into an electron beam vacuum coating instrument, adjusting the template to a first deposition angle, and performing integral metal material evaporation on the chiral structure with the first deposition angle;
step three, performing inclined film coating by adopting a second deposition angle; the third step specifically comprises: adjusting the deposition angle of the template with the chiral structure to a second deposition angle, and performing partial metal material evaporation on the chiral structure with the second deposition angle; the angle of the first deposition angle is greater than the angle of the second deposition angle;
and step four, processing to obtain the chiral structure.
2. The method for preparing the three-dimensional chiral structure with the height difference as claimed in claim 1, wherein the step one, the template preparation of the chiral structure, comprises the following specific steps:
(1) preparing a substrate, and coating a layer of photoresist on the substrate;
(2) designing a structural pattern, and exposing a corresponding area by using an electron beam to form the designed pattern;
(3) soaking the exposed substrate in a developing solution;
(4) and (3) fixing the dried substrate, and drying by using nitrogen to obtain the template with the chiral structure.
3. The method for preparing a three-dimensional chiral structure having a difference in height according to claim 2, wherein: the substrate is ITO glass.
4. The method for preparing the three-dimensional chiral structure with the height difference as claimed in claim 1, wherein the step four of processing to obtain the chiral structure comprises the following specific steps: and (3) putting the template with the chiral structure of the metal material after evaporation into stripping liquid for soaking, performing lift-off stripping process, drying by using nitrogen, and performing SEM observation.
5. A method of preparing a three-dimensional chiral structure having a difference in height according to claim 1, wherein: the coating film is made of gold, silver or copper.
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| CN110531446B (en) * | 2019-09-05 | 2021-03-09 | 陕西师范大学 | U-shaped structure for realizing circular dichroism and preparation method thereof |
| CN111188011B (en) * | 2020-02-17 | 2021-12-24 | 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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| 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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