CN110531446A - A kind of U-shaped structure and preparation method thereof for realizing circular dichroism - Google Patents
A kind of U-shaped structure and preparation method thereof for realizing circular dichroism Download PDFInfo
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- 238000002983 circular dichroism Methods 0.000 title claims abstract description 32
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- 238000005516 engineering process Methods 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 230000008021 deposition Effects 0.000 claims abstract description 15
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- 239000011521 glass Substances 0.000 claims description 11
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- 238000001035 drying Methods 0.000 claims description 7
- 238000001771 vacuum deposition Methods 0.000 claims description 7
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- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 239000010970 precious metal Substances 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 16
- 229910052751 metal Inorganic materials 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 14
- 238000000609 electron-beam lithography Methods 0.000 abstract description 5
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention relates to micronano optical technical fields, more particularly to a kind of U-shaped structure and preparation method thereof for realizing circular dichroism, the structure is formed by connecting by the identical periodic unit plane of multiple structures, it include a U-shaped structure unit in each periodic unit, each structural unit includes horizontal body I, horizontal body II, perpendicular body, one end of horizontal body I is vertical with one end of perpendicular body to be connect, and one end of horizontal body II is vertical with the other end of perpendicular body to be connect, and horizontal body I, horizontal body II, perpendicular body be not in the same horizontal plane.First micro-nano structure template is prepared using electron beam lithography, then by rotary template substrate counterclockwise, and change that electron beam evaporation deposition, tilt angle, the plated film time of evaporation coating are prepared with different height difference chiral metal nanostructure in glancing angle deposition technology.The present invention has different height difference chiral metal nanostructure, and method is simple, at low cost, can be applied to biological monitoring, enantiomer sensing, polarization conversion and photoelectronic circuit polarizer.
Description
Technical field
The present invention relates to micronano optical technical fields, and in particular to a kind of U-shaped structure for realizing circular dichroism and its preparation
Method.
Background technique
A chiral etymology indicates 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 cannot 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
It is all chiral molecules.
Chiral molecules chiral signal in nature is generally very weak.In recent years, researcher's discovery can use chiral gold
Belong to the surface phasmon that nanostructure generates to realize the enhancing of chiral signal.Helical structure can produce annular electro due to it
Stream, so that magnetic direction is parallel in threaded interior direction of an electric field, so as to generate very strong chiral electromagnetic field.But In
It is relatively difficult experimentally directly to prepare helical structure.The chiral nanostructure of three-dimensional with difference in height is similar to spiral, therefore
It can produce stronger chiral signal.However, it has been reported that the three-dimensional chiral nanostructure about preparation with difference in height
Step is not easy relative to the preparation step of helical structure, and long preparation period, and input cost is high.
Summary of the invention
In order to solve the problems in the existing technology, the present invention utilizes electron beam lithography and glancing angle deposition technology
Combination be prepared for different height difference chiral metal U-shaped nano structure.
The invention is realized by the following technical scheme:
A kind of U-shaped structure for realizing circular dichroism, the structure are formed by connecting by the identical periodic unit plane of multiple structures;Institute
Stating each periodic unit includes a U-shaped structure unit;Each structural unit includes horizontal body I, horizontal body II, perpendicular body;Institute
The one end for stating horizontal body I vertical with one end of the perpendicular body is connect;One end of the horizontal body II is vertical with the other end of the perpendicular body
Connection;The horizontal body I, horizontal body II, perpendicular body are not at same level;The horizontal body I, horizontal body II, perpendicular body are by noble metal material
Material Au is made.
Further, the equal length of the horizontal body I and horizontal body II and the perpendicular body;The horizontal body I and horizontal body II and institute
The width for stating perpendicular body is equal;The height of the perpendicular body is greater than the height of the horizontal body I, and the height of the horizontal body II is greater than the cross
The height of body I and the perpendicular body.
Further, realize the preparation method of the U-shaped structure of circular dichroism, which is characterized in that it is described the preparation method is as follows:
Step 1, prepare substrate: preparing ito glass substrate and clean drying;
Step 2, resist coating: photoresist spinner spin coating photoresist PMMA in substrate glasses is utilized;
Step 3, it dries: the substrate of step 2 coating PMMA photoresist being placed on hot plate and is dried;
Step 4, electron beam exposure structure graph: square structure array is designed on pattern generator, and uses electron beam exposure
Technology is exposed figure to substrate obtained in step 3, the substrate after being exposed;When exposure, electron beam is to the structure
The PMMA photoresist of visuals perform etching;
Step 5, develop: under room temperature, the substrate exposed in step 4 being put into impregnate in developer solution and is developed;
Step 6, it is fixed: step 5 being impregnated to the substrate after development and is put into fixing solution and impregnates fixing, takes substrate after the completion of fixing
Out, with being dried with nitrogen;
Step 7, it dries: step 6 being impregnated after being fixed and the substrate of drying is placed on hot plate and dries;
Step 8, gold-plated preparation: the substrate dried after being fixed in step 7 is adhered on coating machine sample stage with vacuum rubber belt, is put
Enter vacuum coating equipment, vacuumizes;Step 9, gold-plated: to rotate counterclockwise formwork structure obtained in step 3 and carry out plated film;Tool
Body process are as follows: in the first filming orientation first along square structure bottom edge, layer of Au is deposited using glancing angle deposition technology;Then inverse
Hour hands are rotated by 90 °, and Au is deposited using glancing angle deposition technology in the second plated film orientation;It is rotated by 90 ° counterclockwise again, in third plated film
Layer of Au is deposited using glancing angle deposition technology in orientation;The time being deposited three times is different, and ultimately forming one has different height
U-shaped structure;The first filming orientation, the second plated film orientation and third plated film orientation are orthogonal;
Step 10, cooling instrument, inflated with nitrogen take out sample.
Step 11, it removes PMMA photoresist: using lift-off technique, the sample that step 10 is taken out steeps in acetone,
Time is no less than 30min, dissolves electron beam PMMA photoresist;
Step 12, dry up: the substrate after drying up the removing PMMA photoresist that step 11 obtains with nitrogen gun obtains the realization circle
Dichromatic U-shaped structure.
Further, the detailed process of the step 1 are as follows: prepare with a thickness of 1.0mm, length and width dimensions be 20.0mm ×
The ito glass of 20.0mm, and the ito glass of preparation is put into cleaning solution and is cleaned, after deionized water ultrasound 15min, with third
Ketone ultrasound 15min, then nitrogen is put into after finally being dried up with nitrogen gun later with deionized water ultrasound 5min with alcohol ultrasound 15min
It is spare in gas holder.
Further, the concrete operations of the step 2 are as follows: set the photoresist spinner whirl coating time as 1 minute, revolving speed 4000
Rpm, it is ensured that substrate surface photoresist forms uniform film.
Further, the concrete operations of the step 3 and step 7 are as follows: hot plate is heated to 150 degrees Celsius, baking time
It is 3 minutes.
Further, the time that development is impregnated in the step 5 is 1 minute.
Further, developer solution from two pentanone of tetramethyl and isopropanol is 3:1 cooperation system with volume ratio in the step 5
At the time for impregnating fixing in the step 7 is 1 minute.
Further, the beginning condition of step 9 plated film is that the chamber pressure of vacuum coating equipment is lower than 3 × 10-6Torr
Compared with prior art, beneficial effects of the present invention:
1, the present invention realizes that the U-shaped structure structure of circular dichroism is simple, can be by between horizontal body I, horizontal body II and the perpendicular body
Simple combination constitute and be similar to three-dimensional spiral structure, to realize strong circular dichroism, structure is simple, and preparation is convenient, is suitble to
Large area production preparation.
2, the present invention realizes that the metal material in the U-shaped structure of circular dichroism can also realize circle two instead of gold using copper
Color reduces the preparation cost of chiral material.
3, the U-shaped structure of the invention for realizing circular dichroism is chiral micro-nano metal structure, and horizontal body I, horizontal body II are erected with described
There is different height difference chiral metal nanostructure between body, can be applied to biological monitoring, enantiomer sensing, polarization conversion and
Photoelectronic circuit polarizer.
Detailed description of the invention
Fig. 1 is the schematic diagram for the U-shaped structure that the present invention realizes circular dichroism.
The step of Fig. 2 is the U-shaped structure of the present invention realization circular dichroism that counterclockwise prepared by rotary template substrate is schemed.
Fig. 3 is the circular dichroism spectrum of the embodiment of the present invention 1.
Fig. 4 is the schematic diagram and its preparation step figure for the E type structure that the embodiment of the present invention 4 realizes circular dichroism.
In figure: 1, the first filming orientation;2, the second plated film orientation;3, third plated film orientation;11, horizontal body I;12, horizontal body II;
13, body is erected.
Specific embodiment
The present invention is described in detail combined with specific embodiments below, but not limited to this.
Embodiment 1:
In order to solve the problems in the existing technology, a kind of U-shaped structure for realizing circular dichroism is present embodiments provided, is utilized
The combination of electron beam lithography and glancing angle deposition technology is prepared for different height difference chiral metal U-shaped nano structure.
The U-shaped structure unit of realization circular dichroism as shown in Figure 1, the structure are connected by the identical periodic unit plane of multiple structures
It forms;Each periodic unit includes a U-shaped structure unit;Each structural unit includes horizontal body I 11, horizontal body II
12, body 13 is erected;One end of the horizontal body I 11 is vertical with one end of the perpendicular body 13 to be connect;One end of the horizontal body II 12 and institute
The other end for stating perpendicular body 13 vertically connects;The horizontal body I 11, horizontal body II 12, perpendicular body 13 be not in the same horizontal plane;The cross
Body I 11, horizontal body II 12, perpendicular body 13 are made of precious metal material Au.
The equal length of the horizontal body I 11 and horizontal body II 12 and the perpendicular body 13;The horizontal body I 11 and horizontal body II 12 and institute
The width for stating perpendicular body 13 is equal;The height of the perpendicular body 13 is greater than the height of the horizontal body I 11, and the height of the horizontal body II 12 is big
In the height of the horizontal body I 11 and the perpendicular body 13.
Specifically: the equal length of horizontal body I 11 and horizontal body II 12 horizontal body II 12 horizontal body II 12 and the perpendicular body 13 is
200nm;The horizontal body I 11 and the II 12 horizontal body II 12 of horizontal body II 12 of horizontal body are equal with the width of the perpendicular body 13, are 40nm;Institute
The height for stating horizontal body I 11 is 40nm, and the height of the perpendicular body 13 is 60nm, and the height of the horizontal body II 1 is 100nm.
As shown in Fig. 2, steps are as follows for the preparation method of the U-shaped structure of above-mentioned realization circular dichroism:
Step 1, prepare substrate: preparing with a thickness of 1.0mm, length and width dimensions are the ito glass of 20.0mm × 20.0mm, and will be prepared
Ito glass be put into cleaning solution and clean, after deionized water ultrasound 15 minutes, with acetone ultrasound 15 minutes, then super with alcohol
It sound 15 minutes, later with deionized water ultrasound 5 minutes, is put into after finally being dried up with nitrogen gun spare in nitrogen cabinet.
Step 2, resist coating: utilizing photoresist spinner spin coating photoresist PMMA in substrate glasses, when setting photoresist spinner whirl coating
Between be 1 minute, 4000 rpm of revolving speed, it is ensured that substrate surface photoresist forms uniform film.
Step 3, it dries: the substrate of step 2 coating PMMA photoresist being placed on the hot plate for having been heated to 150 DEG C, is dried
The roasting time is 3 minutes;Hot plate is placed on ultra-clean indoor ventilation, and dust granules are few herein, is conducive to the volatilization of organic matter, heat
The temperature accuracy of plate is ± 1 DEG C.
Step 4, electron beam exposure structure graph: square structure array is designed with pattern generator, and uses electron beam exposure
Figure, when exposure, electron beam performs etching the PMMA photoresist of the visuals of the structure;Scanning electron microscope exposure
Voltage selects 15KV, and spot selection 5.0,300 μ c/cm2 (microcoulomb is every square centimeter) of exposure dose, step pitch selects 10nm, electricity consumption
Beamlet exposure figure, the substrate after being exposed.
Step 5, develop: under room temperature, the substrate exposed in step 4 being put by two pentanone of tetramethyl and isopropanol with body
Product cooperates in manufactured developer solution than 3:1 impregnates development, and developer solution takes out from -15 DEG C of refrigerators to be used at once at room temperature, is shown
The shadow time controls at Time constant 1 minute;In the case where developing time determines, the precision and exposure dose of figure are linear, and 1 point
400 μ c/cm2 (microcoulomb is every square centimeter) of exposure dose is best when clock.
Step 6, it is fixed: step 5 being impregnated to the substrate after development and is put into fixing solution and impregnates fixing, wherein fixing solution is different
Propyl alcohol;Substrate is taken out after the completion of fixing, with being dried with nitrogen.
Step 7, it dries: step 6 being impregnated to the substrate after being fixed and dried up and is placed on 150 DEG C of hot plate and is dried 3 minutes;Heat
Plate is placed on ultra-clean indoor ventilation, and dust granules are few herein, is conducive to the volatilization of organic matter, and the temperature accuracy of hot plate is ±
1℃。
Step 8, gold-plated preparation: the substrate dried after being fixed in step 7 is adhered to coating machine sample stage with vacuum rubber belt
On, it is put into vacuum coating equipment, is vacuumized;
Step 9, gold-plated: to rotate counterclockwise formwork structure obtained in step 3 and carry out plated film;Detailed process are as follows: first
Layer of Au is deposited using glancing angle deposition technology first along square structure bottom edge in plated film orientation 1;Then it is rotated by 90 ° counterclockwise, In
Au is deposited using glancing angle deposition technology in second plated film orientation 2;It is rotated by 90 ° counterclockwise again, utilizes inclination in third plated film orientation 3
Layer of Au is deposited in angle deposition technique;The time being deposited three times is different, ultimately forms the U-shaped structure with different height.The
One plated film orientation 1, the second plated film orientation 2 and third plated film orientation 3 are orthogonal, the first filming orientation 1, the second plated film orientation 2
It is in same level with third plated film orientation 3, and is mutually in 90 degree, the first filming orientation 1, the second plated film orientation 2 and the
Three plated film orientation 3 are towards inside square structure.
Specifically: the beginning condition of plated film is that the chamber pressure of vacuum coating equipment is lower than 3 × 10-6Torr, vacuum coating
Press proof sample platform and vapor deposition line at it is certain be specially 15 ° ~ 60 °, the process of plated film counterclockwise are as follows: first along square structure bottom
Side utilizes the Au of glancing angle deposition technology vapor deposition 40nm thickness;Then it is rotated by 90 °, along square structure left side, utilizes counterclockwise
The Au of glancing angle deposition technology vapor deposition 60nm thickness;It is rotated by 90 ° counterclockwise again, along square structure top, utilizes glancing angle deposition
The Au of technology vapor deposition 100nm thickness;Ultimately form the U-shaped structure with different height.
Step 10, cooling instrument, inflated with nitrogen take out sample.
Step 11, it removes PMMA photoresist: using lift-off technique, the sample that step 10 is taken out steeps in acetone,
Because acetone is as organic solvent, volatile, toxic, sealed soak is needed, soaking time is at least 30 minutes, dissolves electron beam
PMMA photoresist.
Step 12, dry up: the substrate after drying up the removing PMMA photoresist that step 11 obtains with nitrogen gun obtains the tool
There are different height difference chiral metal nanostructure, i.e., the described U-shaped structure for realizing circular dichroism.
The preparation method kind of above structure, using electron beam lithography exposure structure graphic procedure, electron beam is to the knot
The PMMA photoresist of the visuals of structure performs etching, and the area of structure graph part is less than the gap section outside structure graph,
Since the process of electron beam lithography is very slow, preparation method of the invention saves the time for exposure of structure graph, mentions
High preparation efficiency.
Embodiment 2:
After the U-shaped structure for completing realization circular dichroism of the invention based on embodiment 1 and step preparation, by using Three-D limited
First method (FEM) software for calculation COMSOL Multiphysics carries out calculating simulation test.Specific setting parameter is as follows:
As shown in Figure 1, each periodic unit size are as follows: long 400 nm × wide 400nm;The size of horizontal body I 11 are as follows: long 200nm ×
Wide 40 nm × thickness 40nm;The size of perpendicular body 13 are as follows: long 200nm × wide 40 nm × thickness 60nm;The size of horizontal I I12 of body are as follows: long
200nm × wide 40 nm × thickness 100nm.As shown in figure 3, being the circular dichroism figure of the embodiment of the present application U-shaped structure.It can be with
See, is there are two biggish CD signal at 720nm and 1540nm in wavelength, size is respectively as follows: 20.69% and 12.66%.Structure
It proves, can produce the electric dipole intersected between the horizontal body of the two of the U-shaped structure and a perpendicular body, thickness difference can provide optics
Phase difference, and then generate CD signal.
Embodiment 3
Preparation step is same as Example 1, and difference is only that metal material used is copper.
Gold, silver and copper are different metal material, and the dielectric coefficient of material is different, then corresponding effective refractive index is different,
The transmission peak valley position of metal micro-nanostructure prepared therefrom is unaffected, but intensity in transmission can be different, and usually gold is better than silver,
Silver is better than copper, and the circular dichroism spectral line that the chiral metal nanostructure prepared with gold, silver, copper acquires out has lesser red indigo plant
It moves;But since metal material gold or copper are realized as circular dichroism mechanism with metal material silver, so the chirality prepared
The circular dichroism spectrogram difference of metal Nano structure is not very big.Therefore, the present embodiment selects copper replacement universal in the prior art
The gold used prepares chiral metal nanostructure, and the preparation cost of chiral metal nanostructure can be effectively reduced.
Embodiment 4
Preparation step is substantially the same manner as Example 1, as shown in figure 4, difference is only that the figure designed in step 4 with pattern generator
Shape is convex shape.
The structure finally prepared is with different height difference E font chiral metal nanostructure.E font chiral metal is received
Rice structure compares U-shaped structure, can produce more complicated electromagnetic coupling in the horizontal direction, bigger circular dichroism may be implemented.
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, In
Under the premise of not departing from present inventive concept, several simple deduction or replace made all shall be regarded as belonging to the protection of invention
Range.
Claims (9)
1. a kind of U-shaped structure for realizing circular dichroism, which is characterized in that the structure is put down by the identical periodic unit of multiple structures
Face is formed by connecting;Each periodic unit includes a U-shaped structure unit;Each structural unit includes horizontal body I
(11), horizontal body II (12), perpendicular body (13);One end of the horizontal body I (11) is vertical with one end of the perpendicular body (13) to be connect;It is described
One end of horizontal body II (12) is vertical with the other end of the perpendicular body (13) to be connect;The horizontal body I (11), horizontal body II (12), perpendicular body
(13) it is not at same level;The horizontal body I (11), horizontal body II (12), perpendicular body (13) are made of precious metal material Au.
2. a kind of U-shaped structure for realizing circular dichroism according to claim 1, which is characterized in that the horizontal body I (11) and
The equal length of horizontal body II (12) and the perpendicular body (13);The horizontal body I (11) and horizontal body II (12) and the perpendicular body (13)
Width is equal;The height of the perpendicular body (13) is greater than the height of the horizontal body I (11), and the height of the horizontal body II (12) is greater than institute
State the height of horizontal body I (11) and the perpendicular body (13).
3. the preparation method of -2 any U-shaped structures for realizing circular dichroism according to claim 1, which is characterized in that described
The preparation method is as follows:
Step 1, prepare substrate: preparing ito glass substrate and clean drying;
Step 2, resist coating: photoresist spinner spin coating photoresist PMMA in substrate glasses is utilized;
Step 3, it dries: the substrate of step 2 coating PMMA photoresist being placed on hot plate and is dried;
Step 4, electron beam exposure structure graph: square structure array is designed on pattern generator, and uses electron beam exposure
Technology is exposed figure to substrate obtained in step 3, the substrate after being exposed;When exposure, electron beam is to the structure
The PMMA photoresist of visuals perform etching;
Step 5, develop: under room temperature, the substrate exposed in step 4 being put into impregnate in developer solution and is developed;
Step 6, it is fixed: step 5 being impregnated to the substrate after development and is put into fixing solution and impregnates fixing, takes substrate after the completion of fixing
Out, with being dried with nitrogen;
Step 7, it dries: step 6 being impregnated after being fixed and the substrate of drying is placed on hot plate and dries;
Step 8, gold-plated preparation: the substrate dried after being fixed in step 7 is adhered on coating machine sample stage with vacuum rubber belt, is put
Enter vacuum coating equipment, vacuumizes;
Step 9, gold-plated: to rotate counterclockwise formwork structure obtained in step 3 and carry out plated film;Detailed process are as follows: first
Layer of Au is deposited using glancing angle deposition technology first along square structure bottom edge in plated film orientation (1);Then it is rotated by 90 ° counterclockwise,
Au is deposited using glancing angle deposition technology in the second plated film orientation (2);It is rotated by 90 ° counterclockwise again, in third plated film orientation (3) benefit
Layer of Au is deposited with glancing angle deposition technology;The time being deposited three times is different, ultimately forms the U-shaped knot with different height
Structure;The first filming orientation (1), the second plated film orientation (2) and third plated film orientation (3) are orthogonal;
Step 10, cooling instrument, inflated with nitrogen take out sample;
Step 11, it removes PMMA photoresist: using lift-off technique, the sample that step 10 is taken out steeps in acetone, the time
No less than 30min dissolves electron beam PMMA photoresist;
Step 12, dry up: the substrate after drying up the removing PMMA photoresist that step 11 obtains with nitrogen gun obtains the realization circle
Dichromatic U-shaped structure.
4. the preparation method of the U-shaped structure according to claim 3 for realizing circular dichroism, which is characterized in that the step 1
Detailed process are as follows: prepare with a thickness of 1.0mm, length and width dimensions are the ito glass of 20.0mm × 20.0mm, and by the ITO of preparation
Glass is put into cleaning solution and cleans, after deionized water ultrasound 15min, with acetone ultrasound 15min, then with alcohol ultrasound 15min,
Deionized water ultrasound 5min is used later, is put into after finally being dried up with nitrogen gun spare in nitrogen cabinet.
5. the preparation method of the U-shaped structure according to claim 4 for realizing circular dichroism, which is characterized in that the step 2
Concrete operations are as follows: set the photoresist spinner whirl coating time as 1 minute, 4000 rpm of revolving speed, it is ensured that substrate surface photoresist is formed
Even film.
6. a kind of preparation method of U-shaped structure for realizing circular dichroism according to claim 5, which is characterized in that described
The concrete operations of step 3 and step 7 are as follows: hot plate is heated to 150 degrees Celsius, baking time is 3 minutes.
7. a kind of preparation method of U-shaped structure for realizing circular dichroism according to claim 6, which is characterized in that described
The time that development is impregnated in step 5 is 1 minute.
8. a kind of preparation method of U-shaped structure for realizing circular dichroism according to claim 7, which is characterized in that described
Developer solution is to be made with 3:1 with volume ratio from two pentanone of tetramethyl and isopropanol in step 5, and fixing is impregnated in the step 7
Time be 1 minute.
9. a kind of preparation method of U-shaped structure for realizing circular dichroism according to claim 8, which is characterized in that described
The beginning condition of step 9 plated film is that the chamber pressure of vacuum coating equipment is lower than 3 × 10-6Torr 。
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