CN114527529B - Preparation method of high-resolution structural color device - Google Patents
Preparation method of high-resolution structural color device Download PDFInfo
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- CN114527529B CN114527529B CN202210151500.XA CN202210151500A CN114527529B CN 114527529 B CN114527529 B CN 114527529B CN 202210151500 A CN202210151500 A CN 202210151500A CN 114527529 B CN114527529 B CN 114527529B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 123
- 238000009966 trimming Methods 0.000 claims abstract description 69
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 63
- 238000004528 spin coating Methods 0.000 claims abstract description 55
- 238000001035 drying Methods 0.000 claims abstract description 53
- 238000000151 deposition Methods 0.000 claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 29
- 239000012782 phase change material Substances 0.000 claims abstract description 27
- 238000000137 annealing Methods 0.000 claims abstract description 26
- 238000005530 etching Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000005507 spraying Methods 0.000 claims description 37
- 239000003292 glue Substances 0.000 claims description 32
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 20
- 230000007246 mechanism Effects 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 238000003860 storage Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- 239000011651 chromium Substances 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 238000010884 ion-beam technique Methods 0.000 claims description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 10
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 10
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000005485 electric heating Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 5
- 238000005566 electron beam evaporation Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052594 sapphire Inorganic materials 0.000 claims description 5
- 239000010980 sapphire Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- 238000004544 sputter deposition Methods 0.000 claims description 5
- 239000013077 target material Substances 0.000 claims description 5
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000007639 printing Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 24
- 238000005520 cutting process Methods 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 6
- 239000003086 colorant Substances 0.000 description 5
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
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- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
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Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1847—Manufacturing methods
- G02B5/1857—Manufacturing methods using exposure or etching means, e.g. holography, photolithography, exposure to electron or ion beams
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0005—Production of optical devices or components in so far as characterised by the lithographic processes or materials used therefor
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/16—Coating processes; Apparatus therefor
- G03F7/162—Coating on a rotating support, e.g. using a whirler or a spinner
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/16—Coating processes; Apparatus therefor
- G03F7/168—Finishing the coated layer, e.g. drying, baking, soaking
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Optics & Photonics (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
Abstract
The invention discloses a preparation method of a high-resolution structural color device, and relates to the technical field of structural color devices. The preparation method comprises the steps of firstly depositing a phase change material on a substrate, and annealing to obtain the substrate with a phase change material film layer; spin-coating photoresist on the upper surface of the phase change material film layer through spin-coating trimming and drying equipment, drying and trimming, transferring a preset super-surface reverse structure pattern onto the photoresist, and developing and exposing to obtain a super-surface structure pattern; depositing a metal film on the pattern of the super-surface structure, and dissolving to obtain a mask structure; and etching the mask structure to remove the residual metal mask material, thereby obtaining the high-resolution structural color device with the super-surface structure. The invention realizes the color display of the structural color device with high resolution, high saturation and wide color gamut, increases the display quality of the structural color of the super surface, and is not easy to damage and fall off; the method is suitable for the technical fields of multifunctional display, CMOS image sensors, ink-free color printing, information encryption and the like.
Description
Technical Field
The invention relates to the technical field of structural color devices, in particular to a preparation method of a high-resolution structural color device.
Background
At present, research on existing structural color devices at home and abroad focuses on improving the saturation, efficiency and wide visual angle of the structural color devices, and only static colors can be provided, namely, once the device structure is prepared, the generated colors are unchanged, and the requirements of the current color display technology cannot be met. The current nano-photon structure for realizing structural color generation mainly comprises a thin film structure based on thin film interference and a grating structure based on guided wave resonance mode. The widely used thin film structure consists of a fabry-perot resonant cavity based on a metal-dielectric-metal three-layer thin film. The structure works in such a way that the output of different colors is realized by changing the thickness of the intermediate medium film. Thus, at least three thin film deposition steps are required to be performed in each case in the preparation of a color pixel array including red, green, blue or cyan, magenta, and yellow. In addition, the thickness of each layer of film needs to be precisely controlled in the preparation process, so that the structural color device is not beneficial to mass production. The structural color device based on the guided wave resonance mode mainly comprises a sub-wavelength diffraction grating, and the resonance wavelength can be regulated and controlled by changing the grating period, so that filtering out of different colors is obtained.
The invention patent of publication number CN112346151a discloses a monocrystalline silicon supersurface for achieving high performance structural colors, comprising an alumina substrate and a monocrystalline silicon supersurface on the alumina substrate, the alumina substrate and the monocrystalline silicon supersurface being encapsulated by an index matching layer. The refractive index matching layer is utilized to realize wide color gamut, high brightness, high saturation and high resolution structural color simultaneously, the preparation difficulty is low, and the application value of the structural color is expanded and improved. However, the following technical problems are found: the display quality of the structural color cannot be further improved through active regulation and control, the device is not easy to damage and fall off, the spin coating and drying efficiency of the photoresist cannot be further improved in the spin coating process, and the distribution uniformity and quality of the photoresist are guaranteed.
Disclosure of Invention
The invention aims to provide a preparation method of a high-resolution structural color device, which is used for solving the technical problems that the display quality of structural color cannot be further improved through active regulation and control, the device is not easy to damage and fall off, the spin-coating drying efficiency of photoresist cannot be further improved in the spin-coating process, and the distribution uniformity and quality of photoresist are ensured in the prior art.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the high-resolution structural color device comprises the following steps:
s1, depositing a phase change material on a substrate, and annealing to obtain the substrate with a phase change material film layer;
s2, spin-coating photoresist on the upper surface of the phase change material film layer through spin-coating trimming and drying equipment, drying and trimming, transferring a preset super-surface reverse structure pattern onto the photoresist, and developing and exposing to obtain a super-surface structure pattern;
s3, depositing a metal film on the pattern of the super-surface structure, and dissolving off to obtain a mask structure;
and S4, etching the mask structure to remove residual metal mask material, and obtaining the high-resolution structural color device with the super-surface structure.
Further, the material of the substrate in the step S1 is selected from one or a mixture of more of silicon, silicon dioxide, silicon carbide, silicon nitride and sapphire; the phase change material is selected from vanadium dioxide.
Further, the step S1 is to adopt a magnetron sputtering deposition method, the target material selected by the magnetron sputtering deposition method is a metal target, the sputtering power is 110-120W, the pressure is 6-8 mTorr, and the growth temperature is 600-610 ℃.
Further, annealing is performed in the step S1 by adopting an annealing furnace under the argon/hydrogen atmosphere, the annealing temperature is 440-455 ℃, the annealing time is 4-5 hours, and the flow rates of the argon and the hydrogen are 75-82 sccm and 3-5 sccm respectively.
Further, the photoresist in the step S2 is selected from polymethyl methacrylate, the rotating speed in spin coating is 4200-4600 rpm, the drying temperature is 175-185 ℃, and the drying time is 1-2 hours; the exposure is performed by using a special developer of polymethyl methacrylate.
Further, in the step S3, the metal film is a chromium film, the dissolved solution is acetone, the electron beam evaporation deposition is adopted for deposition, and the thickness of the mask structure is 20-30 nm.
Further, in the step S4, ion beam etching is adopted, the energy of the ion beam is 300eV, etching gas is argon, and the pressure is 18-21 mTorr; and removing the residual metal mask material by adopting chromium corrosive liquid.
Further, the spin coating trimming and drying equipment performs spin coating photoresist, drying and trimming as follows:
photoresist spin coating: placing a plurality of substrates with phase change material film layers in a containing groove of a substrate placing table, and vacuumizing a rotating table through a vacuum tube by a vacuum pump, wherein the vacuum tube is also vacuumized, so that the substrates are adsorbed; the first motor drives the glue spraying box to rotate through the connecting shaft, so that the glue spraying head moves to the upper part of the substrate placing table, photoresist in the glue storage box is sprayed to the substrate on the corresponding substrate placing table through the glue spraying head, and the electric motor drives the rotary table and the substrate to finish rotary spraying in the process of rotating;
and (3) drying: turning off the vacuum pump, turning on the blower, blowing air into the heating cavity by the blower through the air supply pipe, heating the air by the electric heating wire to form hot air at 175-185 ℃, blowing the hot air into the outer surface of the substrate through the accommodating groove, and drying the photoresist for 1-2 hours;
trimming: the second motor drives the driving belt pulley to rotate, the driving belt pulley further drives the driving belt and the driven belt pulley to rotate, and the driven belt pulley drives the rotary box body to rotate through the rotary shaft, so that the substrate placing table rotates to a position close to the ball screw;
the third motor drives the ball screw to rotate, the screw rod seat in threaded connection with the ball screw moves along the axial direction of the ball screw, the screw rod seat drives the clamping seat and the trimming seat to move up and down, when the clamping seat and the trimming seat move to a proper position, the piston shaft of the telescopic cylinder drives the trimming seat to move towards the substrate placing table until the trimming knife moves to the edge position of the substrate, and the third motor drives the trimming knife to be attached to the edge of the substrate; the electric motor drives the rotary table to rotate, so that the substrate moves relative to the trimming knife, and the trimming knife cuts off redundant photoresist at the edge of the substrate.
Further, the spin coating, trimming and drying equipment comprises a spin coating box body, a photoresist spin coating and drying mechanism and a trimming mechanism are arranged in the inner cavity of the spin coating box body, the photoresist spin coating and drying mechanism comprises a spin box body and a photoresist spraying box, a plurality of substrate placing tables are arranged on the upper surface of the spin box body, a concave containing groove is formed in the center of each substrate placing table, a substrate is placed on the upper surface of each containing groove, a rotary table is arranged at the bottom of each containing groove, a plurality of adsorption tubes communicated with the corresponding containing grooves are arranged in a cavity of the rotary table, a heating cavity is formed between the rotary table and each substrate placing table, and electric heating wires are arranged in the heating cavity; the center top of spouting the gluey case is connected with first motor through the connecting axle, spouts the upper surface of gluey case and is equipped with the storage gluey case, spouts the lower surface of gluey case and is equipped with a plurality of spouts gluey heads that correspond with the substrate platform of placing.
Further, the plurality of substrate placing tables are distributed on the upper surface of the rotary box body in an annular array, and the plurality of glue spraying heads are distributed on the lower surface of the glue spraying box in an annular array; the lower surface of the rotary box body is fixedly provided with a blower and a vacuum pump, the blower is communicated with the wall part of the heating cavity through a plurality of air supply pipes, the vacuum pump is used for pumping vacuum to the inner cavity of the rotary table through a plurality of vacuum pipes, and a gap is reserved between the vacuum pipes and the rotary table.
The invention has the following beneficial effects:
1. according to the preparation method of the high-resolution structural color device, the phase change material is deposited on the substrate, the optical property of the phase change material is adjustable, the device has the structural color which is dynamically adjustable under external excitation such as electricity and heat, and the active regulation and control of the structural color of the device are realized; the super surface structure pattern obtained by developing exposure can completely absorb light with a certain wavelength and has unique transmission/reflection characteristics, so that color display with high resolution, high saturation and wide color gamut is realized, and the highest resolution exceeds 100,000dpi; the mask structure obtained by depositing a metal film and dissolving off increases the structural color display quality of the super surface, and is not easy to damage and drop off; the method is suitable for the technical fields of multifunctional display, CMOS image sensors, ink-free color printing, information encryption and the like.
2. The preparation method completes synchronous spin coating and drying of a plurality of substrates through spin coating and trimming drying equipment, and trims in time, thereby improving the spin coating and drying efficiency of the substrates and the uniformity and quality of photoresist distribution.
3. The spin coating trimming and drying equipment is used for placing a substrate through a plurality of substrate placing tables on the upper surface of the rotary box body, the substrate is firmly adsorbed after vacuum is extracted from the plurality of adsorption pipes, and after the electric heating wires in the heating cavity are electrified and heated, heat is blown into the outer surface of the substrate through the accommodating groove for high-efficiency drying; the first motor drives the glue spraying box to rotate through the connecting shaft, so that the glue spraying head moves to the upper side of the substrate placing table, photoresist in the glue storage box is sprayed to the corresponding substrate on the substrate placing table through the glue spraying head, the rotary spraying operation is completed in the process that the rotary table drives the substrate to rotate, and redundant photoresist at the edge of the substrate is cut through the edge cutting mechanism.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view of a spin-on trimming and drying apparatus in an embodiment of the present invention;
FIG. 2 is a cross-sectional view of a rotary housing according to an embodiment of the present invention;
FIG. 3 is an enlarged view of a portion of the invention at A in FIG. 2;
FIG. 4 is a schematic structural view of a trimming mechanism according to an embodiment of the present invention;
FIG. 5 is a three-dimensional view of a trimming mechanism in accordance with an embodiment of the present invention;
FIG. 6 is a top view of a rotary case according to an embodiment of the present invention;
fig. 7 is a bottom view of the glue spraying box according to the embodiment of the invention.
In the figure: 10. spin coating the box body; 20. rotating the box body; 21. a substrate placement stage; 22. a receiving groove; 23. a substrate; 24. a rotary table; 25. an adsorption tube; 26. a heating chamber; 27. a heating wire; 28. an annular groove; 29. a support column; 30. a glue spraying box; 31. a connecting shaft; 32. a first motor; 33. a glue storage box; 34. a glue spraying head; 35. a rubber conveying pipe; 36. an electromagnetic flow regulating valve; 37. an electric motor; 40. a blower; 41. a vacuum pump; 42. an air supply pipe; 43. a vacuum tube; 44. a second motor; 45. a driving pulley; 46. a driven pulley; 47. a drive belt; 48. a rotation shaft; 50. a third motor; 51. a ball screw; 52. a telescopic cylinder; 53. a bearing seat; 54. a fixed rod; 55. a screw rod seat; 56. a clamping seat; 57. a piston shaft; 58. cutting edge seats; 59. a trimming shaft; 60. and (5) trimming a knife.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a preparation method of a high-resolution structural color device, which comprises the following steps:
s1, depositing a phase change material on a substrate, and annealing to obtain the substrate with a phase change material film layer; wherein the material of the substrate is selected from one or more of silicon, silicon dioxide, silicon carbide, silicon nitride and sapphire; the phase change material is selected from vanadium dioxide; the deposition adopts a magnetron sputtering deposition method, the target material selected by the magnetron sputtering deposition method is a metal target, the sputtering power is 112W, the pressure is 6.8mTorr, and the growth temperature is 605 ℃; annealing is performed in an argon/hydrogen atmosphere by adopting an annealing furnace, the annealing temperature is 446 ℃, the annealing time is 4.2 hours, and the flow rates of argon and hydrogen are 78sccm and 3.5sccm respectively.
S2, spin-coating photoresist on the upper surface of the phase change material film layer through spin-coating trimming and drying equipment, drying and trimming, transferring a preset super-surface reverse structure pattern onto the photoresist, and developing and exposing to obtain a super-surface structure pattern; wherein the photoresist is selected from polymethyl methacrylate, the rotating speed is 4300rpm during spin coating, the drying temperature is 180 ℃, and the drying time is 1.5 hours; the exposure is performed by using a special developer of polymethyl methacrylate.
S3, depositing a metal film on the pattern of the super-surface structure, and dissolving off to obtain a mask structure; the metal film is a chromium film, the dissolved solution is acetone, the deposition is carried out by electron beam evaporation, and the thickness of the mask structure is 22nm.
And S4, etching the mask structure to remove residual metal mask material, and obtaining the high-resolution structural color device with the super-surface structure. The etching adopts ion beam etching, the energy of the ion beam is 300eV, the etching gas is argon, and the pressure is 20mTorr; and removing the residual metal mask material by adopting chromium corrosive liquid.
Example 2
The embodiment provides a preparation method of a high-resolution structural color device, which comprises the following steps:
s1, depositing a phase change material on a substrate, and annealing to obtain the substrate with a phase change material film layer; wherein the material of the substrate is selected from one or more of silicon, silicon dioxide, silicon carbide, silicon nitride and sapphire; the phase change material is selected from vanadium dioxide; the deposition adopts a magnetron sputtering deposition method, the target material selected by the magnetron sputtering deposition method is a metal target, the sputtering power is 115W, the pressure is 6.8mTorr, and the growth temperature is 608 ℃; annealing is performed in an argon/hydrogen atmosphere by adopting an annealing furnace, the annealing temperature is 450 ℃, the annealing time is 4.6 hours, and the flow rates of argon and hydrogen are respectively 80sccm and 4.2sccm.
S2, spin-coating photoresist on the upper surface of the phase change material film layer through spin-coating trimming and drying equipment, drying and trimming, transferring a preset super-surface reverse structure pattern onto the photoresist, and developing and exposing to obtain a super-surface structure pattern; wherein the photoresist is selected from polymethyl methacrylate, the rotating speed during spin coating is 4500rpm, the drying temperature is 182 ℃, and the drying time is 1.5 hours; the exposure is performed by using a special developer of polymethyl methacrylate.
S3, depositing a metal film on the pattern of the super-surface structure, and dissolving off to obtain a mask structure; the metal film is a chromium film, the dissolved solution is acetone, the deposition is carried out by electron beam evaporation, and the thickness of the mask structure is 26nm.
And S4, etching the mask structure to remove residual metal mask material, and obtaining the high-resolution structural color device with the super-surface structure. The etching adopts ion beam etching, the energy of the ion beam is 300eV, the etching gas is argon, and the pressure is 19mTorr; and removing the residual metal mask material by adopting chromium corrosive liquid.
Example 3
The embodiment provides a preparation method of a high-resolution structural color device, which comprises the following steps:
s1, depositing a phase change material on a substrate, and annealing to obtain the substrate with a phase change material film layer; wherein the material of the substrate is selected from one or more of silicon, silicon dioxide, silicon carbide, silicon nitride and sapphire; the phase change material is selected from vanadium dioxide; the deposition adopts a magnetron sputtering deposition method, the target material selected by the magnetron sputtering deposition method is a metal target, the sputtering power is 120W, the pressure is 7.6mTorr, and the growth temperature is 608 ℃; annealing is performed in an argon/hydrogen atmosphere by adopting an annealing furnace, the annealing temperature is 452 ℃, the annealing time is 4.8 hours, and the flow rates of argon and hydrogen are 82sccm and 5sccm respectively.
S2, spin-coating photoresist on the upper surface of the phase change material film layer through spin-coating trimming and drying equipment, drying and trimming, transferring a preset super-surface reverse structure pattern onto the photoresist, and developing and exposing to obtain a super-surface structure pattern; wherein the photoresist is selected from polymethyl methacrylate, the rotating speed is 4600rpm when in spin coating, the drying temperature is 178 ℃, and the drying time is 2 hours; the exposure is performed by using a special developer of polymethyl methacrylate.
S3, depositing a metal film on the pattern of the super-surface structure, and dissolving off to obtain a mask structure; the metal film is a chromium film, the dissolved solution is acetone, the deposition is carried out by electron beam evaporation, and the thickness of the mask structure is 28nm.
And S4, etching the mask structure to remove residual metal mask material, and obtaining the high-resolution structural color device with the super-surface structure. The etching adopts ion beam etching, the energy of the ion beam is 300eV, the etching gas is argon, and the pressure is 21mTorr; and removing the residual metal mask material by adopting chromium corrosive liquid.
Example 4
As shown in fig. 1-3 and fig. 6-7, the present embodiment provides a spin-coating, trimming and drying apparatus, which is used for completing the photoresist spin-coating, drying and trimming processes in the process of preparing high-resolution structural color devices, and comprises a spin-coating box 10, wherein a photoresist spin-coating and drying mechanism and a trimming mechanism are arranged in an inner cavity of the spin-coating box 10. Specifically, photoresist spin-coating stoving mechanism includes rotatory box 20, spouts gluey case 30, and rotatory box 20's upper surface is equipped with a plurality of substrates and places platform 21, and the center that the platform 21 was placed to the substrate is equipped with indent storage tank 22, and substrate 23 has been placed to storage tank 22 upper surface, and the bottom of storage tank 22 is equipped with revolving stage 24, is equipped with many adsorption tubes 25 with storage tank 22 intercommunication in the cavity of revolving stage 24, is equipped with heating chamber 26 between revolving stage 24 and the substrate placing platform 21, is equipped with electric heater strip 27 in the heating chamber 26. The center top of spouting gluey case 30 is connected with first motor 32 through connecting axle 31, and spouts gluey case 30's upper surface and is equipped with the storage gluey case 33, spouts gluey case 30's lower surface and is equipped with a plurality of spouts gluey heads 34 that correspond with substrate placement table 21.
In the spin coating, trimming and drying equipment of the embodiment, a substrate 23 is placed by a plurality of substrate placing tables 21 on the upper surface of a rotary box body 20, the substrate 23 is firmly adsorbed after vacuum is extracted from a plurality of adsorption pipes 25, and after an electric heating wire 27 in a heating cavity 26 is electrified and heated, heat is blown into the outer surface of the substrate 23 through a containing groove 22 for drying; the first motor 32 drives the photoresist spraying box 30 to rotate through the connecting shaft 31, so that the photoresist spraying head 34 moves to the upper side of the substrate placing table 21, photoresist in the photoresist storage box 33 is sprayed to the substrate 23 on the corresponding substrate placing table 21 through the photoresist spraying head 34, the rotary spraying operation is completed in the process that the rotary table 24 drives the substrate 23 to rotate, and redundant photoresist at the edge of the substrate 23 is cut off through the edge cutting mechanism. The spin-coating trimming and drying equipment can finish synchronous spin-coating and drying of a plurality of substrates 23, timely trim edges, and improves spin-coating drying efficiency of the substrates 23 and uniformity and quality of photoresist distribution.
The lower surface of the rotary table 24 is connected with an electric motor 37 for driving the rotary table 24 and the substrate 23 to rotate, the lower surface of the rotary box 20 is provided with an annular groove 28, and the inner cavity of the rotary box 20 is provided with a support column 29 which is in sliding connection with the annular groove 28. In the process of driving the rotary table 24 and the substrate 23 to rotate by the electric motor 37, the glue spraying head 34 sprays onto the upper surface of the substrate 23 to finish spin coating; when the rotary case 20 is driven to rotate, the annular groove 28 slides relative to the support column 29, and the support column 29 provides a supporting force for the rotary case 20, thereby ensuring stable rotation of the rotary case 20.
The plurality of substrate placement tables 21 are distributed on the upper surface of the rotary box body 20 in an annular array, and the plurality of glue spraying heads 34 are distributed on the lower surface of the glue spraying box 30 in an annular array. A blower 40 and a vacuum pump 41 are fixed to the lower surface of the rotary casing 20, the blower 40 communicates with the wall of the heating chamber 26 through a plurality of air pipes 42, the vacuum pump 41 pumps vacuum to the inner chamber of the rotary table 24 through a plurality of vacuum pipes 43, and a gap is provided between the vacuum pipes 43 and the rotary table 24. The blower 40 blows air into the heating chamber 26 through the air supply pipe 42, the electric heating wire 27 heats the air to form hot air, and the hot air is blown into the outer surface of the substrate 23 through the accommodating groove 22 to dry the photoresist. The vacuum pump 41 draws vacuum to the turntable 24 through the vacuum tube 43, and the suction tube 25 is also drawn vacuum, so that the substrate 23 is firmly sucked.
The inner cavity of the rotary box body 20 is provided with a second motor 44, a motor shaft of the second motor 44 extends vertically upwards, the periphery of the motor shaft is connected with a driving belt pulley 45, a driven belt pulley 46 is arranged below the center of the rotary box body 20, the driving belt pulley 45 and the periphery of the driven belt pulley 46 are tightly tensioned, a transmission belt 47 is arranged on the periphery of the driving belt pulley 45, and the axis center of the driven belt pulley 46 is connected with a rotary shaft 48 extending into the center of the rotary box body 20. After the second motor 44 is started, the driving pulley 45 is driven to rotate, the driving pulley 45 further drives the driving belt 47 and the driven pulley 46 to rotate, and the driven pulley 46 drives the rotary box 20 to rotate, so that the position of the substrate placing table 21 can be regulated stably.
The glue storage tank 33 is connected with a glue feeding pipe 35 extending into the inner cavity of the glue spraying tank 30, and an electromagnetic flow regulating valve 36 is connected between the glue spraying head 34 and the lower surface of the glue spraying tank 30. The photoresist in the photoresist storage tank 33 flows into the inner cavity of the photoresist spraying tank 30 through the rubber delivery pipe 35, and the electromagnetic flow regulating valve 36 is used for precisely regulating and controlling the photoresist amount sprayed by the photoresist spraying head 34.
As shown in fig. 1 and fig. 4-5, two edge cutting mechanisms are symmetrically arranged on two sides above the rotary box body 20, and comprise a third motor 50, a ball screw 51 and a telescopic cylinder 52, wherein the third motor 50 is fixed on the top of the inner cavity of the rotary box body 10, the third motor 50 is connected with the ball screw 51 which extends vertically downwards through a coupling, the periphery of the bottom end of the ball screw 51 is connected with a bearing seat 53, the periphery of the bearing seat 53 is connected with a fixing rod 54 connected with the inner wall of the rotary box body 10, the periphery of the ball screw 51 is in threaded connection with a screw seat 55, one side, facing the inner cavity of the rotary box body 10, of the screw seat 55 is connected with a clamping seat 56, the telescopic cylinder 52 is clamped in the clamping seat 56, a piston shaft 57 of the telescopic cylinder 52 is connected with an edge cutting seat 58, the center of the edge cutting seat 58 is provided with an edge cutting shaft 59 in a penetrating way, and the bottom end of the edge cutting shaft 59 is connected with an edge cutter 60.
The cross-sectional shape of the trimming blade 60 matches the cross-sectional shape of the substrate 23, for example, when the cross-section of the substrate 23 is circular, the cross-section of the trimming blade 60 is semicircular, and when the cross-section of the substrate 23 is rectangular, the cross-section of the trimming blade 60 is elongated.
After the photoresist on the surface of the substrate 23 is dried, driving the rotary box 20 to enable the substrate placing table 21 to rotate to a position close to the ball screw 51, driving the ball screw 51 to rotate by the third motor 50, axially moving a screw rod seat 55 in threaded connection with the ball screw 51 along the ball screw 51, driving a clamping seat 56 and a trimming seat 58 to move up and down by the screw rod seat 55, driving the trimming seat 58 to move towards the substrate placing table 21 by a piston shaft 57 of the telescopic cylinder 52 until the trimming blade 60 moves to the edge position of the substrate 23 when the trimming mechanism moves to a proper position, and driving the trimming blade 60 to be attached to the edge of the substrate 23 by the third motor 50; after the electric motor 37 is turned on, the electric motor 37 drives the rotary table 24 to rotate, so that the substrate 23 moves relative to the trimming blade 60, and the trimming blade 60 cuts off the excessive photoresist on the edge of the substrate 23. The trimming mechanism can realize the transverse and longitudinal position adjustment of the trimming blade 60, and trim the edges according to the shape of the substrate 23, so as to keep the uniform distribution of the photoresist on the surface of the substrate 23.
As shown in fig. 1 to 7, the spin-coating trimming and drying apparatus of the present embodiment works as follows:
photoresist spin coating: placing a plurality of substrates 23 in the accommodation groove 22 of the substrate placement table 21, vacuum pumping 41 pumping vacuum to the turntable 24 through vacuum pipes 43, suction pipe 25 also pumping vacuum, so that the substrates 23 are sucked; the first motor 32 drives the glue spraying box 30 to rotate through the connecting shaft 31, so that the glue spraying head 34 moves to the upper part of the substrate placing table 21, photoresist in the glue storage box 33 is sprayed to the substrate 23 on the corresponding substrate placing table 21 through the glue spraying head 34, and the electric motor 37 drives the rotary table 24 and the substrate 23 to finish rotary spraying in the process of rotating;
and (3) drying: turning off the vacuum pump 41, turning on the blower 40, blowing air into the heating cavity 26 by the blower 40 through the air supply pipe 42, heating the air by the electric heating wire 27 to form hot air with the temperature of 175-185 ℃, blowing the hot air into the outer surface of the substrate 23 through the accommodating groove 22, and drying the photoresist for 1-2 hours;
trimming: the second motor 44 drives the driving pulley 45 to rotate, the driving pulley 45 further drives the driving belt 47 and the driven pulley 46 to rotate, and the driven pulley 46 drives the rotary case 20 to rotate through the rotary shaft 48, so that the substrate placing table 21 rotates to a position close to the ball screw 51;
the third motor 50 drives the ball screw 51 to rotate, the screw rod seat 55 in threaded connection with the ball screw 51 moves axially along the ball screw 51, the screw rod seat 55 drives the clamping seat 56 and the trimming seat 58 to move up and down, when the clamping seat 56 and the trimming seat 58 move to a proper position, the piston shaft 57 of the telescopic cylinder 52 drives the trimming seat 58 to move towards the substrate placing table 21 until the trimming blade 60 moves to the edge position of the substrate 23, and the third motor 50 drives the trimming blade 60 to be attached to the edge of the substrate 23; the electric motor 37 drives the rotary table 24 to rotate so that the substrate 23 moves relative to the trimming blade 60, and the trimming blade 60 cuts off the excess photoresist at the edge of the substrate 23.
The foregoing is merely illustrative of the structures of this invention and various modifications, additions and substitutions for those skilled in the art can be made to the described embodiments without departing from the scope of the invention or from the scope of the invention as defined in the accompanying claims.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (8)
1. The preparation method of the high-resolution structural color device is characterized by comprising the following steps of:
s1, depositing a phase change material on a substrate, and annealing to obtain the substrate with a phase change material film layer;
s2, spin-coating photoresist on the upper surface of the phase change material film layer through spin-coating trimming and drying equipment, drying and trimming, transferring a preset super-surface reverse structure pattern onto the photoresist, and developing and exposing to obtain a super-surface structure pattern;
s3, depositing a metal film on the pattern of the super-surface structure, and dissolving off to obtain a mask structure;
s4, etching the mask structure to remove residual metal mask material, and obtaining a high-resolution structural color device with a super-surface structure;
the spin coating trimming and drying equipment performs spin coating photoresist, drying and trimming as follows:
photoresist spin coating: placing a plurality of substrates with phase change material film layers in a containing groove (22) of a substrate placing table (21), and vacuumizing a rotating table (24) through a vacuum pipe (43) by a vacuum pump (41), wherein a vacuum is also pumped by an adsorption pipe (25), so that the substrates are adsorbed; the first motor (32) drives the glue spraying box (30) to rotate through the connecting shaft (31), so that the glue spraying head (34) moves to the upper part of the substrate placing table (21), photoresist in the glue storage box (33) is sprayed to a substrate on the corresponding substrate placing table (21) through the glue spraying head (34), and the electric motor (37) drives the rotary table (24) to finish rotary spraying in the process of rotating the substrate;
and (3) drying: closing a vacuum pump (41), starting a blower (40), blowing air into the heating cavity (26) by the blower (40) through an air supply pipe (42), heating the air by an electric heating wire (27) to form hot air at 175-185 ℃, blowing the hot air into the outer surface of the substrate through a containing groove (22), and drying the photoresist for 1-2 hours;
trimming: the second motor (44) drives the driving belt pulley (45) to rotate, the driving belt pulley (45) further drives the transmission belt (47) and the driven belt pulley (46) to rotate, and the driven belt pulley (46) drives the rotary box body (20) to rotate through the rotary shaft (48) so that the substrate placing table (21) rotates to a position close to the ball screw (51);
the third motor (50) drives the ball screw (51) to rotate, the screw rod seat (55) in threaded connection with the ball screw (51) moves axially along the ball screw (51), the screw rod seat (55) drives the clamping seat (56) and the trimming seat (58) to move up and down, when the clamping seat and the trimming seat move to a proper position, the piston shaft (57) of the telescopic cylinder (52) drives the trimming seat (58) to move towards the substrate placing table (21) until the trimming knife (60) moves to the edge position of the substrate, and the third motor (50) drives the trimming knife (60) to be attached to the edge of the substrate; an electric motor (37) drives the rotary table (24) to rotate, so that the substrate moves relative to the edge trimming cutter (60), and the edge trimming cutter (60) cuts off redundant photoresist at the edge of the substrate;
the spin coating, trimming and drying equipment comprises a spin coating box body (10), a photoresist spin coating and drying mechanism and a trimming mechanism are arranged in the inner cavity of the spin coating box body (10), the photoresist spin coating and drying mechanism comprises a spin box body (20) and a photoresist spraying box (30), a plurality of substrate placing tables (21) are arranged on the upper surface of the spin box body (20), a concave containing groove (22) is formed in the center of the substrate placing tables (21), a substrate (23) is arranged on the upper surface of the containing groove (22), a rotary table (24) is arranged at the bottom of the containing groove (22), a plurality of adsorption tubes (25) communicated with the containing groove (22) are arranged in the cavity of the rotary table (24), a heating cavity (26) is formed between the rotary table (24) and the substrate placing tables (21), and electric heating wires (27) are arranged in the heating cavity (26); the center top of spouting gluey case (30) is connected with first motor (32) through connecting axle (31), and the upper surface of spouting gluey case (30) is equipped with storage gluey case (33), and the lower surface of spouting gluey case (30) is equipped with a plurality of spouts gluey heads (34) that correspond with substrate placement platform (21).
2. The method for manufacturing a high resolution structural color device according to claim 1, wherein the substrate in step S1 is made of a material selected from one or more of silicon, silicon dioxide, silicon carbide, silicon nitride, and sapphire; the phase change material is selected from vanadium dioxide.
3. The method for manufacturing the high-resolution structural color device according to claim 1, wherein the step S1 is a magnetron sputtering deposition method, the target material selected by the magnetron sputtering deposition method is a metal target, the sputtering power is 110-120W, the pressure is 6-8 mTorr, and the growth temperature is 600-610 ℃.
4. The method for manufacturing a high-resolution structural color device according to claim 1, wherein the annealing in step S1 is performed by an annealing furnace under an argon/hydrogen atmosphere, the annealing temperature is 440-455 ℃, the annealing time is 4-5 hours, and the flow rates of argon and hydrogen are 75-82 sccm and 3-5 sccm, respectively.
5. The method for manufacturing a high resolution structural color device according to claim 1, wherein the photoresist in step S2 is selected from polymethyl methacrylate, the spin-coating speed is 4200-4600 rpm, the baking temperature is 175-185 ℃, and the baking time is 1-2 hours; the exposure is performed by using a special developer of polymethyl methacrylate.
6. The method for manufacturing a high-resolution structural color device according to claim 1, wherein the metal film in the step S3 is a chromium film, the dissolved solution is acetone, the deposition is electron beam evaporation deposition, and the thickness of the mask structure is 20-30 nm.
7. The method for manufacturing a high-resolution structural color device according to claim 1, wherein in the step S4, ion beam etching is adopted, the energy of the ion beam is 300eV, the etching gas is argon, and the pressure is 18-21 mTorr; and removing the residual metal mask material by adopting chromium corrosive liquid.
8. The method for manufacturing the high-resolution structural color device according to claim 1, wherein the plurality of substrate placement tables (21) are distributed on the upper surface of the rotary box body (20) in an annular array, and the plurality of glue spraying heads (34) are distributed on the lower surface of the glue spraying box (30) in an annular array; a blower (40) and a vacuum pump (41) are fixed on the lower surface of the rotary box body (20), the blower (40) is communicated with the wall part of the heating cavity (26) through a plurality of blast pipes (42), the vacuum pump (41) is used for vacuumizing the inner cavity of the rotary table (24) through a plurality of vacuum pipes (43), and a gap is reserved between the vacuum pipes (43) and the rotary table (24).
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