CN109375306B - Method for manufacturing cholesteric liquid crystal polymer sheet - Google Patents
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Abstract
The invention discloses a method for manufacturing cholesteric liquid crystal polymer slices, which utilizes a microfluidic centrifugal technology to realize the production of PCLC (cholesteric liquid crystal polymer) slices in batch and continuity, the microfluidic technology can operate, process and control micro fluid in a micro channel, and the method has the advantages of simple process, small loss, integrated miniaturization, fast response and the like, overcomes the uncontrollable property of slice shape, and improves the defects of poor reusability and low efficiency of a mould.
Description
Technical Field
The invention relates to the field of liquid crystal optics, in particular to a method for manufacturing a cholesteric liquid crystal polymer sheet.
Background
Cholesteric liquid crystal Polymer (PCLC) flakes were developed in the 90's of the 20 th century with good properties to replace cholesteric liquid crystals and PCLC thin films with lower molar masses. The cholesteric liquid crystal molecules are susceptible to the action of an electric field or a magnetic field, so that controllability of optical properties can be realized. Since cholesteric liquid crystal molecules are extremely temperature sensitive, small temperature changes can change their properties, even causing phase changes, into a solid or liquid state. If liquid crystal molecules are incorporated into long polymer chains to form PCLC thin films, their temperature sensitivity can be reduced. Since the PCLC thin film has a very strong viscosity property, a good alignment effect can be achieved only in a very small area, which severely limits the application of the PCLC thin film. The PCLC thin sheet combines the properties of the micromolecular cholesteric liquid crystal and the PCLC thin film, not only has temperature stability and alignment uniformity, but also keeps photoelectric controllability. The PCLC flake has a special molecular spiral structure, so that the PCLC flake has unique selective reflection and Bragg-type effect. Selective reflection, namely: the PCLC platelet surface can only cause reflection of light of a specific wavelength and (circular) polarization. When the sight deviates from the direction of the screw axis of the sheet or the incident light forms an included angle with the screw axis, the selective reflection wavelength moves towards short wave, so that the reflected light disappears, and further, an obvious visual effect is generated. The PCLC sheet can also be used for producing right (left) chiral circularly polarized light, and 3D effects and safety guarantee functions such as identification, anti-counterfeiting and the like are easy to realize. The good properties of redirection, coordination, selective reflection and temperature stability of the PCLC sheet make the PCLC sheet have immeasurable application value in the aspects of commerce and science.
To date, several tens to several hundreds of micrometers of PCLC flakes are produced mainly by the following methods:
physical fracture method: the PCLC thin film was physically broken up to form small PCLC flakes. The broken flakes have both the important optical properties of liquid crystals and remain temperature insensitive. The method mostly adopts mechanical crushing, the size and the shape of the thin slice are difficult to control, and the regularity research and the finished product production are limited. The technical scheme of the physical fracture method is as follows: US5364557, U.S. patent database publication, and CN103351704B, chinese patent database publication.
Soft etching template method: mainly coating a large amount of Polydimethylsiloxane (PDMS) on a patterned silicon wafer until solidification and stripping are carried out, forming a patterned PDMS mold, filling the PDMS mold with PCLC, aligning, detecting, cooling, and finally bending the mold to extrude a PCLC sheet. Although the uncertain factor of uncontrollable shape of a physical fracture method is improved by the soft etching template method, the structure of the die is easily damaged by bending an extruded sheet by the method, and the reusability of the die is poor. The technical scheme of the soft etching template method is as follows: US20040173927 published by US patent database.
In addition, the two methods can not realize continuous batch production, greatly reduce the production efficiency and limit the application of industrialization and integration.
Disclosure of Invention
The invention provides a method for manufacturing a cholesteric liquid crystal Polymer (PCLC) sheet, which overcomes the defects of the method for manufacturing the PCLC sheet in the background technology.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a method of making a cholesteric liquid crystal polymer sheet comprising:
the method comprises the following steps that (1) a microfluidic centrifugal chip with a centrifugal channel with gradually reduced depth is manufactured, a liquid storage tank is arranged in the center of the chip, and a sample outlet is formed in the edge of the microfluidic centrifugal chip;
step (2) preparing monodisperse cholesteric liquid crystal polymer liquid drops with uniform size by using a liquid drop preparation device;
centrifuging the cholesteric liquid crystal polymer liquid drops injected into the liquid storage tank of the microfluidic centrifugal chip through a centrifugal channel with the depth smaller than the diameter of the liquid drops by using the centrifugal effect to form flat liquid drops;
and (4) polymerizing the flat liquid drops which are centrifuged to the outermost centrifugal channel in the step (4) by illumination to form a cholesteric liquid crystal polymer sheet, and outputting the cholesteric liquid crystal polymer sheet from a sample outlet of the microfluidic centrifugal chip.
In one embodiment: in the step (1), the microfluidic centrifugal chip comprises a substrate and a cover plate, a liquid storage tank is arranged in the center of the substrate, a centrifugal channel with the depth decreasing from inside to outside is arranged on the periphery of the substrate, a sample outlet is communicated with the centrifugal channel, and a sample inlet capable of being communicated with the liquid storage tank is arranged in the center of the cover plate.
In one embodiment: the centrifugal channel is an annular channel surrounding the liquid storage tank, or a linear channel taking the liquid storage tank as a center and radially distributed from the center to the periphery, or a spiral channel taking the liquid storage tank as a center.
In one embodiment: in the step (2), the cholesteric liquid crystal polymer droplet component comprises cholesteric liquid crystal, an initiator and a monomer.
In one embodiment: the cholesteric liquid crystal is selected from one or more of cholesterol acetate, cholesterol propionate, cholesterol n-butyrate, cholesterol pelargonate, cholesterol oleate, cholesteryl linoleate, cholesterol benzoate, cholesterol cinnamate, cholesterol ethyl carbonate, cholesterol oleyl carbonate, cholesteryl isostearyl carbonate, cholesteryl butenoate, cholesteryl carbonate and cholesterol chloride.
In one embodiment: the cholesteric liquid crystal can be prepared by doping a nematic liquid crystal with a chiral agent.
In one embodiment: in the step (2), when the cholesteric liquid crystal polymer liquid drops are prepared, the inner phase is a liquid crystal mixture, the outer phase is a material immiscible with the liquid crystal mixture, and the flow rates of the inner phase and the outer phase are controlled to obtain the monodisperse cholesteric liquid crystal polymer liquid drops with uniform sizes.
In one embodiment: the external phase material which is not mutually soluble with the liquid crystal mixture is selected from one or more of aqueous phase solution, glycerin, silicone oil and paraffin oil.
In one embodiment: in said step (4), the thickness of the cholesteric liquid crystal polymer flakes is equal to the depth of the outermost centrifugal channels.
Compared with the background technology, the technical scheme has the following advantages:
in order to overcome the defects of the two methods, the invention provides a novel method for manufacturing PCLC sheets, which realizes the continuous production of PCLC sheets in batches by using a microfluidic centrifugation technology, wherein the microfluidic technology can operate, process and control micro fluid (such as nano-liter to pico-liter) in a micro channel, and can produce the following technical effects: the method has the advantages of simple process, low loss, integrated miniaturization, quick response and the like; secondly, the uncontrollable property of the shape of the thin sheet is overcome, and the defects of poor reutilization property and low efficiency of the die are overcome; thirdly, the edge of the PCLC flake is smoothly deformed with curvature instead of artificial mechanical truncation, which has profound significance for researching the optical property of the PCLC flake; fourthly, the micro-fluidic can realize the manufacture of PCLC thin sheets with the diameter of tens to hundreds of microns.
Drawings
FIG. 1 is a diagram of an apparatus for making a cholesteric liquid crystal polymer sheet.
Fig. 2 is a top view of a microfluidic chip substrate.
Fig. 3 is a side view of a microfluidic chip substrate.
Figure 4 is a top view of a microfluidic chip cover plate.
FIG. 5(a) is a pictorial representation of a cholesteric liquid crystal polymer sheet under a polarizing microscope using wet etching;
FIG. 5(b) is a schematic diagram of a cholesteric liquid crystal polymer sheet under a polarizing microscope using an inductively coupled plasma etching method.
The labels in the figure are: 1.1-polymerization light source, 1.2-sample introduction device, 1.3-sample introduction port, 1.4-centrifugal channel, 1.5-cover plate, 1.6-substrate, 1.7-centrifugal drive module, 1.8-sample introduction port, 2.1-liquid storage tank, 2.2-support column, 2.3-side view cutting line and 3.3-cover plate through hole.
Detailed Description
The following will further describe an embodiment of a method for producing a cholesteric liquid crystal Polymer (PCLC) sheet with reference to the accompanying table and drawings.
Example one
A method of making a cholesteric liquid crystal Polymer (PCLC) platelet comprising:
the microfluidic centrifugal chip with the centrifugal channel gradually reduced in depth is manufactured in the step (1), the chip comprises a substrate and a cover plate, a liquid storage tank is arranged in the center of the substrate, the centrifugal channel with the gradually reduced depth from inside to outside is arranged on the periphery of the substrate, a sample outlet communicated with the centrifugal channel is formed in the edge of the substrate, and a sample inlet communicated with the liquid storage tank is formed in the center of the cover plate; the centrifugal channel is an annular channel surrounding the liquid storage tank, or a linear channel taking the liquid storage tank as a center and radially distributed from the center to the periphery, or a spiral channel taking the liquid storage tank as a center.
Preparing monodisperse PCLC liquid drops with uniform size by using a liquid drop preparation device;
centrifuging the PCLC liquid drops injected into the liquid storage tank of the microfluidic centrifugal chip by using the centrifugal effect to pass through a centrifugal channel with the depth smaller than the diameter of the liquid drops to form flat liquid drops;
and (4) polymerizing the flat liquid drops which are centrifuged to the outermost ring polymerization channel by illumination to form a PCLC sheet, and collecting the PCLC sheet. In the step (4), one or more light sources for illumination polymerization may be selected.
The droplet preparation device in the step (2) can be integrated with the microfluidic centrifugal chip in the step (1).
In the first embodiment: the step (1) comprises the following steps:
step 1-1, manufacturing a substrate 1.6;
step 1-2, making a cover plate 1.5;
and 1-3, rinsing the cover plate 1.5 and the substrate 1.6 by using a Polyethylene (PVA) aqueous solution, for example rinsing by using a 4-6 wt% Polyethylene (PVA) aqueous solution for 1-3min, specifically selecting 5 wt% and 2min, and then attaching the two together by using a clamp to finish the manufacture of the microfluidic chip.
The specific implementation method for manufacturing the substrate 1.6 in the step 1-1 comprises the following steps: selecting a circular glass plate with the diameter of 40cm and the thickness of 2cm as a substrate 1.6, etching a ring of channels with the gradient depth change from inside to outside on a glass plate substrate by utilizing wet etching and controlling the corrosion time of an acid solution on glass, wherein the depth of the channels is equidistantly reduced from inside to outside, and the specific operation process is as follows: first, the substrate 1.6 is wrapped with a corrosion-resistant material (e.g., tape), and then a laser lithography machine is used to etch a designed pattern on one side of the glass plate, as shown in fig. 2, the width of the outermost ring of the equal-depth ring pattern is about 6cm, the ring width of each of the other inner rings is about 3cm, and three support pillars 2.2 are further provided on the substrate 1.6, the three support pillars 2.2 are located in the outermost ring, and the diameter of the support pillars 2.2 is about 2 cm. Etching with an acid solution containing HF and HNO3，HF:HNO3The acid solution ratio is: HF: HNO3:H2O is 9-11:6-8:80-90, specifically 10:7:83 (volume ratio), and the etching rate is 1-1.5um/min, specifically 1.2 um/min. By controlling time variable, annular channels with equal gradient depth change are etched from inside to outside, the annular channels form a gradient ring 1.4, and the depth of the channels decreases equidistantly from inside to outside to enable the height of the gradient ring 1.4 to be gradually increased from inside to outside. The specific operation method is, for example: the inner ring is stripped and carved, and the outermost ring is protected and supported from acid liquid. The etch depth of each ring is shown in table 1 and the side view of the substrate 1.6 is shown in fig. 3.
Table 1, the correspondence between the number of wet-etched rings and the etching depth.
| Number of rings | Etch depth (μm) |
| 1 | 150 |
| 2 | 130 |
| 3 | 115 |
| 4 | 100 |
| 5 | 85 |
| 6 | 60 |
The specific implementation method for manufacturing the cover plate 1.5 in the step 1-2 comprises the following steps: a circular organic glass with the diameter of 55cm and the thickness of 1cm is selected as a cover plate 1.5, a through hole 3.3 with a proper size is engraved at a position corresponding to the center of a circle of the cover plate 1.5 by using a laser photoetching method, and the corresponding position is shown in figure 4.
The liquid storage tank 2.1 with the deepest depth is formed at the position of the corresponding circle center of the substrate 1.6, the liquid storage tank 2.1 is aligned with the through hole 3.3 of the cover plate to form a sample inlet 1.3, and PCLC liquid drops are added into the chip through the sample inlet 1.3. The outer circumferential wall of the substrate 1.6 is provided with a sample outlet 1.8 which is connected to the gradient ring 1.4. The centrifugal channel is provided with a polymerization channel positioned at the outermost ring, and the thickness of the PCLC thin sheet is equal to the depth of the polymerization channel.
The cover plate and the substrate can be one or more of quartz glass, metal, Polydimethylsiloxane (PDMS), polymethyl methacrylate (PMMA), polytetrafluoroethylene, polycarbonate and polystyrene. The etching method of the substrate and the cover plate selects one or more of wet etching, soft imprinting etching, inductively coupled plasma etching (ICP), optical etching, hot imprinting etching, excimer etching and 3D printing according to different materials. The substrate and the cover plate can be processed respectively and then bonded; the base sheet and the cover sheet can also be integrally injection molded.
The step (2) is specifically as follows: monodisperse PCLC droplets of uniform size were prepared, which consisted of 74 wt% cholesteric liquid crystal (96.8 wt% nematic liquid crystal E7 and 3.2 wt% chiral agent R5011), 1 wt% initiator 651 and 25 wt% monomer system, where the monomer system consisted of RM 257: RM 82: RM 006: RM 021: RM010 ═ 3: 2: 2: 2: 1 (mass ratio). The inner phase is liquid crystal cholesteric liquid crystal polymer solution, the outer phase is 10 wt% PVA water solution, and the flow rate of the inner phase and the outer phase is controlled to obtain the PCLC liquid drop with the diameter of 100-150 μm, such as 120 μm, which is uniformly monodisperse. In the step (2), the cholesteric liquid crystal polymer droplet component comprises cholesteric liquid crystal, an initiator and a monomer. The cholesteric liquid crystal is selected from one or more of cholesterol acetate, cholesterol propionate, cholesterol n-butyrate, cholesterol pelargonate, cholesterol oleate, cholesteryl linoleate, cholesterol benzoate, cholesterol cinnamate, cholesterol ethyl carbonate, cholesterol oleyl carbonate, cholesteryl isostearyl carbonate, cholesteryl butenoate, cholesteryl carbonate and cholesterol chloride. The cholesteric liquid crystal can be prepared by doping a nematic liquid crystal with a chiral agent. The nematic liquid crystal is selected from one or more of E7, E12, 5CB, E48, ZLI4788, ZLI2293, BL006, BL036, MDA-00-3461, MDA-00-3506 and MLC 6608. The chiral agent is selected from one or more of S811, R811, S5011, R1011, CB15, BDH1281, BP-CD3, COC and MLC 6248. The initiator is selected from one or more of Irgacure 651, Irgacure 1173, Irgacure184, Irgacure 127, Irgacure 784, Irgacure 819, Irgacure 2202, Irgacure 2959 and Chemcure-481. The monomer is selected from one or more of RM257, RM82, RM84, RM006, RM021, RM010, RM206, RM691, C6M, BAHB, SLC1717, LC242, M1 and M2.
The step (3) and the step (4) specifically comprise the following steps:
step A, fixing the microfluidic chip, the feeding device 1.2, the polymerization light source 1.1 and the centrifugal driving module 1.7 on an iron stand bracket in sequence according to the positions shown in figure 1.
Step B, adding enough PCLC drops into the feeding device 1.2, filling the liquid storage tank 1.3, turning on the polymerization light source 1.1, setting the wavelength at 350nm and the illumination intensity at 96mw/cm2；
And step C, placing a circular ring-shaped receiving device on the outer side of the micro-fluidic chip, taking 5 wt% of Polyethylene (PVA) aqueous solution contained in the device as a substrate, starting centrifugal drive, driving the micro-fluidic chip to rotate by the centrifugal drive module 1.7, setting the rotating speed to be 500rpm/s, centrifuging the PCLC liquid drop to form a flat liquid drop, carrying out illumination polymerization on the flat liquid drop which is centrifuged to the outermost ring polymerization channel to form a PCLC sheet, finally separating the PCLC sheet from the sample outlet 1.8 and dropping the PCLC sheet into the circular ring receiving device, and collecting and obtaining a batch of PCLC sheets.
A physical representation under a polarizing microscope of a PCLC sheet after centrifugal polymerization is shown in FIG. 5 (a).
Example two
It differs from the first embodiment in that: the specific implementation method for manufacturing the substrate 1.6 in the step 1-1 comprises the following steps: a circular quartz glass plate with the diameter of 50cm and the thickness of 2cm is selected as a substrate 1.6, an Inductively Coupled Plasma (ICP) etching technology is adopted, a ring-shaped channel with the gradient depth change is etched on a quartz glass substrate 1.6, and the specific experimental process comprises the following steps: wrapping the substrate 1.6 with an anti-corrosion adhesive tape, and then etching a circular ring pattern on the adhesive tape on one side of the glass plate by using a laser photoetching machine, wherein the pattern is as shown in figure 2, the width of the outermost ring of the circular pattern with equal depth is about 5cm, the width of each of the rest rings is about 3cm, and the diameter of three support columns in the outermost ring is about 2 cm; placing the quartz substrate in an ICP-2B type etching machine, and etching with F12For etching gases, RF1Power 300w, RF2The power is 100w, the pressure is 0.35Pa, the gas flow is 35ml/min, and the etching rate of the quartz material under the room temperature condition is 42 nm/min. By controlling the time variable, the annular channel with the equal gradient depth change is etched from inside to outside to form a gradient ring 1.4. The specific operation method comprises the steps of stripping a ring in the inner ring and etching the ring, and the outermost ring is supported and not etched. The etch depth of each ring is shown in Table 2, and the side view of the substrate 1.6 is shown in FIG. 3Shown in the figure.
TABLE 2 inductively coupled plasma etch, number of rings versus etch depth
| Number of rings | Etch depth (μm) |
| 1 | 200 |
| 2 | 175 |
| 3 | 160 |
| 4 | 145 |
| 5 | 130 |
| 6 | 115 |
| 7 | 100 |
| 8 | 85 |
A physical representation under a polarizing microscope of a PCLC sheet after centrifugal polymerization is shown in FIG. 5 (b).
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.
Claims (8)
1. A method of making a cholesteric liquid crystal polymer sheet, characterized by: the method comprises the following steps:
the method comprises the following steps that (1) a microfluidic centrifugal chip with a centrifugal channel with gradually reduced depth is manufactured, a liquid storage tank is arranged in the center of the chip, and a sample outlet is formed in the edge of the microfluidic centrifugal chip;
preparing monodisperse cholesteric liquid crystal polymer liquid drops by using a liquid drop preparation device;
centrifuging the cholesteric liquid crystal polymer liquid drops injected into the liquid storage tank of the microfluidic centrifugal chip through a centrifugal channel with the depth smaller than the diameter of the liquid drops by using the centrifugal effect to form flat liquid drops;
and (4) polymerizing the flat liquid drops which are centrifuged to the outermost centrifugal channel in the step (4) by illumination to form a cholesteric liquid crystal polymer sheet, and outputting the cholesteric liquid crystal polymer sheet from a sample outlet of the microfluidic centrifugal chip.
2. A method of manufacturing a cholesteric liquid crystal polymer sheet according to claim 1, wherein: in the step (1), the microfluidic centrifugal chip comprises a substrate and a cover plate, a liquid storage tank is arranged in the center of the substrate, a centrifugal channel with the depth decreasing from inside to outside is arranged on the periphery of the substrate, a sample outlet is communicated with the centrifugal channel, and a sample inlet capable of being communicated with the liquid storage tank is arranged in the center of the cover plate.
3. A method of manufacturing a cholesteric liquid crystal polymer sheet according to claim 1 or 2, wherein: the centrifugal channel is an annular channel surrounding the liquid storage tank, or a linear channel taking the liquid storage tank as a center and radially distributed from the center to the periphery, or a spiral channel taking the liquid storage tank as a center.
4. A method of manufacturing a cholesteric liquid crystal polymer sheet according to claim 1, wherein: in the step (2), the cholesteric liquid crystal polymer droplet component comprises cholesteric liquid crystal, an initiator and a monomer.
5. A method of manufacturing a cholesteric liquid crystal polymer sheet according to claim 4, wherein: the cholesteric liquid crystal is selected from one or more of cholesterol acetate, cholesterol propionate, cholesterol n-butyrate, cholesterol pelargonate, cholesterol oleate, cholesteryl linoleate, cholesterol benzoate, cholesterol cinnamate, cholesterol ethyl carbonate, cholesterol oleyl carbonate, cholesteryl isostearyl carbonate, cholesteryl butenoate, cholesteryl carbonate and cholesterol chloride.
6. A method of manufacturing a cholesteric liquid crystal polymer sheet according to claim 4, wherein: the cholesteric liquid crystal can be prepared by doping a nematic liquid crystal with a chiral agent.
7. A method of manufacturing a cholesteric liquid crystal polymer sheet according to claim 6, wherein: the nematic liquid crystal is selected from one or more of E7, E12, 5CB, E48, ZLI4788, ZLI2293, BL006, BL036, MDA-00-3461, MDA-00-3506 and MLC 6608.
8. A method of manufacturing a cholesteric liquid crystal polymer sheet according to claim 1, wherein: in said step (4), the thickness of the cholesteric liquid crystal polymer flakes is equal to the depth of the outermost centrifugal channels.
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| US5364557A (en) * | 1991-11-27 | 1994-11-15 | Faris Sades M | Aligned cholesteric liquid crystal inks |
| US7238316B2 (en) * | 2003-03-07 | 2007-07-03 | University Of Rochester | Method for making precisely configured flakes useful in optical devices |
| CN103752358B (en) * | 2014-01-23 | 2015-07-15 | 西南科技大学 | Polymer micro-fluidic chip and preparation method thereof |
| CN106113128B (en) * | 2016-06-23 | 2018-07-31 | 湖北祥源新材科技股份有限公司 | A kind of polymer flake, manufacturing method and application |
| CN107151558B (en) * | 2017-04-20 | 2020-09-22 | 广东工业大学 | Polymer stabilized liquid crystal and preparation method thereof |
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