CN105218717A - A kind of ultraviolet step-by-step polymerization prepares the method for wide band photomasking film material - Google Patents
A kind of ultraviolet step-by-step polymerization prepares the method for wide band photomasking film material Download PDFInfo
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Abstract
Utilize ultraviolet step-by-step polymerization to prepare a method for wide band photomasking film material, belong to liquid crystal material field.Nematic liquid crystal, chipal compounds, ultraviolet free radical polymerization monomer, ultraviolet free radical photo-initiation, ultraviolet cationically polymerizable monomers and ultraviolet cation light initiator are mixed according to certain mass ratio, makes the cholesteric liquid crystal compound system that pitch increases with the rising of temperature.By the ultraviolet light irradiation of 365nm under low temperature, ultraviolet free radical polyalcohol network is made to fix pitch less in compound system, at high temperature adopt the ultraviolet light irradiation compound system of 254nm, ultraviolet cationic polymers network is made to fix the larger pitch of another part, the non-uniform Distribution of pitch is formed by ultraviolet step-by-step polymerization, thus the wide band photomasking film material of obtained heat, light outfield accuracy controlling.Advantage of the present invention is that manufacture craft is simple, and accuracy controlling, can be used for the wide band photomasking film material of different-waveband requirement.
Description
Technical field
The invention belongs to field of application of liquid crystal, provide a kind of method that ultraviolet step-by-step polymerization prepares wide band photomasking film material.This material can be widely used in the field such as liquid-crystal display light brightness enhancement film, building doors and windows adhering film to glass or coating and military affairs infrared stealth shielding material.
Background technology
Cholesteryl phase (N* phase) liquid crystal is one of liquid crystal material found the earliest, is also the liquid crystal material applied at present widely simultaneously.Its formation condition mainly contains two kinds, and a kind of have chiral structure for liquid crystal molecule itself, and two is the chipal compounds that adulterates in nematic liquid crystal.Due to the existence of chiral structure, under intermolecular special interaction, make N* phase liquid crystal have periodic helical arrangement mode, its distance required for liquid crystal molecule rotating 360 degrees is called pitch (P).For the N* phase liquid crystal that nematic liquid crystal doping chipal compounds is formed, the chipal compounds of its doping different sorts and content can produce different impacts to the pitch of N* phase liquid crystal, P=1/ (HTP × X
c), wherein HTP is the helical twisting power of chipal compounds, X
cfor the molar fraction of chipal compounds in liquid crystal.Therefore, when chipal compounds content is certain, the helical twisting power of chipal compounds is larger, and the pitch of N* phase liquid crystal is less.
N* phase liquid crystal has the characteristic of selective reflection incident light, and its wavelength reflected the incident light is λ=nP, and the wavelength width reflected the incident light is Δ λ=Δ nP, and wherein n and Δ n is respectively mean refractive index and the birefringence index of N* phase liquid crystal material.In reflection wavelength width, the circularly polarized light identical with cholesteric liquid crystal spirane structure rotation direction is reflected, and contrary with cholesteric liquid crystal spirane structure rotation direction or outside reflection bandwidth circularly polarized light is transmitted away.Generally speaking, for colourless organic materials, the numerical value of its Δ n is generally less than 0.3, and in visible region, the reflection wave of N* phase liquid crystal is wide is about 100nm.If think to increase reflection wave wide region further, according to formula Δ λ=Δ nP, it is more feasible for increasing pitch, and method conventional is at present that pitch in N* phase liquid crystal compound system is formed Gradient distribution or non-uniform Distribution.
Reflection for different-waveband range incident light effectively can realize the effect shielding different-waveband incident light, and reflected waveband scope can be applied to the light brightness enhancement film etc. of the liquid-crystal display of energy-conserving and environment-protective at the N* phase liquid crystal composite material of visible region; Reflected waveband scope can be applied to the building doors and windows adhering film to glass or coating etc. of energy-conserving and environment-protective at the N* phase liquid crystal composite material near infrared light region; Reflected waveband scope can be applied to the infrared stealth shielding material etc. of military field at the N* phase liquid crystal composite material in mid-infrared light region.Therefore, wide band photomasking film material has important application prospect at numerous areas, thus has attracted the extensive concern of numerous Chinese scholars.Nineteen ninety-five, Holland scientist D.J.Broer teaches the principle of research group (CN97191106.1) by molecular diffusion, according to the character of dye absorber UV-light, form ultraviolet ray intensity gradient in film thickness direction, and then prepare the N* phase liquid crystal laminated film with pitch gradient distribution.Wide wave reflective film prepared by them can reflect the circularly polarized light of whole visible wavelength range.Because the diffusion of monomer in liquid crystal is relevant with ultraviolet ray intensity, therefore the ripple that formed of this method is wide very responsive to UV intensity, need in the fabrication process to use monochromatic ray sensor to detect polaroid, its technics comparing is complicated, more difficult control.
Summary of the invention
The object of the present invention is to provide a kind of making method of simple wide band photomasking film material, raw material is simple and easy to get, and technique is simple, and cost is lower.
Prepare the method for wide band photomasking film material with ultraviolet step-by-step polymerization, its concrete preparation technology is:
Step 1: nematic liquid crystal, chipal compounds, ultraviolet free radical polymerization monomer, ultraviolet free radical photo-initiation, ultraviolet cationically polymerizable monomers and ultraviolet cation light initiator are mixed according to certain mass ratio, wherein the weight percent of nematic liquid crystal is: 40 ~ 90%; The weight percent of chipal compounds is: 1 ~ 10%; The weight percent of ultraviolet free radical polymerization monomer is: 1 ~ 20%; The weight percent of ultraviolet free radical photo-initiation is: 0.1 ~ 10%; The weight percent of ultraviolet cationically polymerizable monomers is: 1 ~ 30%; 0.1 ~ 10% of the weight percent of ultraviolet cation light initiator, is heated to isotropy state by mixture, with oscillator vibrates repeatedly, mix, there is the transformation of isotropy state-cholesteryl phase in cooling, i.e. the cholesteric liquid crystal compound system of obtained mixture, lucifuge in operating process.
Step 2: the cholesteric liquid crystal compound system of step 1 mixture is circulated in advance in the liquid crystal cell of planar orientation process, the thickness of liquid crystal cell is 10 ~ 100 μm; To the liquid crystal cell after process first in the temperature range of 0 ~ 40 DEG C, employing wavelength is the ultraviolet light irradiation 5 ~ 100min of 365nm, and ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2ultraviolet free radical polymerization monomer is polymerized, fix 30 ~ 50% scopes fine pitch (the pitch scope of 0 ~ 40 DEG C 0.1 ~ 1.0 μm), then by thermal station, compound system is heated, in another temperature range of 40 ~ 100 DEG C, employing wavelength is the ultraviolet light irradiation 5 ~ 100min of 254nm, and ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2, ultraviolet cationically polymerizable monomers is polymerized, fixes the coarse pitch (the pitch scope of 40 ~ 100 DEG C 1.0 ~ 3.0 μm) of 50 ~ 70% scopes.
Step 3: by regulating the chiral compound substrate concentration in cholesteric liquid crystal, can prepare correspond to can reflect visible light district optical band or the cholesteryl phase mixed system of reflect near IR district optical band, carry out ultraviolet light irradiation again, make UV-light polymerisable monomer step-by-step polymerization, ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2.
Further, described chipal compounds comprises the one in binaphthol, 4 '-(2-methyl butyl)-4-biphenyl cyanogen, Isosorbide and derivative thereof, its helical twisting power reduces along with the increase of temperature, and the pitch of the cholesteric liquid crystal compound system of mixture increases along with the increase of temperature.
Further, described ultraviolet free radical polymerization monomer is one or several in esters of acrylic acid, methyl acrylic ester, vinylbenzene base class, diacetyl base class, and active function groups quantity is 1 ~ 5.
Further, described ultraviolet free radical photo-initiation is benzoin dimethylether IRG651.
Further, ultraviolet cationically polymerizable monomers is one or several in flexible chain redix or stiff chain redix, and active function groups quantity is 1 ~ 5.
Further, ultraviolet cation light initiator is two (4-tert.-butylbenzene) iodine hexafluorophosphates.
Further, the internal surface of described liquid crystal cell is through planar orientation process, and planar orientation is treated to rubbing manipulation, Vacuum Coating method or chemical method.
The invention has the advantages that: the wide band photomasking film material that can realize heat, light outfield accuracy controlling, the material source that this kind of thin-film material uses enriches, and manufacture craft is simple, easily accomplishes scale production.And this thin-film material can be according to actual needs, by changing the concentration of chipal compounds, come the position at accommodation reflex center, Application and preparation in liquid-crystal display light brightness enhancement film (reflect visible light region) or be applied to the infrared stealth shielding material (reflection mid-infrared light region) of energy-conservation environment protection architecture windowpane pad pasting or coating (reflect near infrared light region) or military field.
Accompanying drawing explanation
Fig. 1 is the transmitted light spectrogram of the liquid-crystal film material that in the embodiment of the present invention 1, sample is tested at 15 DEG C, and curve 1 is the transmitted light spectrogram before sample 1 is polymerized; Curve 2 is the transmitted light spectrograms after sample 1 is polymerized, and polymerizing condition is: 15 DEG C, 365nm, 2mW/cm
2irradiation 10 minutes, then 60 DEG C, 254nm, 2mW/cm
2irradiation 10 minutes; Curve 3 is the transmitted light spectrograms after sample 1 is polymerized, and polymerizing condition is: 15 DEG C, 365nm, 2mW/cm
2irradiation 10 minutes, then 60 DEG C, 254nm, 2mW/cm
2irradiation 20 minutes; Curve 4 is the transmitted light spectrograms after sample 1 is polymerized, and polymerizing condition is: 15 DEG C, 365nm, 2mW/cm
2irradiation 10 minutes, then 60 DEG C, 254nm, 2mW/cm
2irradiation 30 minutes.
Fig. 2 is the transmitted light spectrogram of the liquid-crystal film material that in the embodiment of the present invention 2, sample is tested at 15 DEG C, and curve 5 is the transmitted light spectrograms before sample 2 is polymerized; Curve 6 is the transmitted light spectrograms after sample 2 is polymerized, and polymerizing condition is: 15 DEG C, 365nm, 2mW/cm
2irradiation 10 minutes, then 60 DEG C, 254nm, 2mW/cm
2irradiation 10 minutes; Curve 7 is the transmitted light spectrograms after sample 2 is polymerized, and polymerizing condition is: 15 DEG C, 365nm, 4mW/cm
2irradiation 10 minutes, then 60 DEG C, 254nm, 4mW/cm
2irradiation 10 minutes; Curve 8 is the transmitted light spectrograms after sample 2 is polymerized, and polymerizing condition is: 15 DEG C, 365nm, 6mW/cm
2irradiation 10 minutes, then 60 DEG C, 254nm, 6mW/cm
2irradiation 10 minutes.
Fig. 3 is the profile scanning electromicroscopic photograph of the macromolecule network that the thin-film material of preparation in the embodiment of the present invention 1 is formed, and as can be seen from the figure, pitch is non-uniform Distribution.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described further.
Prepare the method for wide band photomasking film material with ultraviolet step-by-step polymerization, its concrete preparation technology is:
Step 1: by nematic liquid crystal, chipal compounds, ultraviolet free radical polymerization monomer, ultraviolet free radical photo-initiation, ultraviolet cationically polymerizable monomers and ultraviolet cation light initiator according to certain mass than mixture, wherein the weight percent of nematic liquid crystal is: 40 ~ 90%; The weight percent of chipal compounds is: 1 ~ 10%; The weight percent of ultraviolet free radical polymerization monomer is: 1 ~ 20%; The weight percent of ultraviolet free radical photo-initiation is: 0.1 ~ 10%; The weight percent of ultraviolet cationically polymerizable monomers is: 1 ~ 30%; 0.1 ~ 10% of the weight percent of ultraviolet cation light initiator.Mixture is heated to isotropy state, with oscillator vibrates repeatedly, mixing, there is the transformation of isotropy state-cholesteryl phase in cooling, i.e. the cholesteric liquid crystal compound system of obtained mixture, lucifuge in operating process.
Step 2: the N* phase liquid crystal compound system of above-mentioned mixture is circulated in advance in the liquid crystal cell of planar orientation process, the thickness of liquid crystal cell is 10 ~ 100 μm, afterwards to liquid crystal cell in the temperature range of 0 ~ 40 DEG C, employing wavelength is the ultraviolet light irradiation 5 ~ 100min of 365nm, and ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2, ultraviolet free radical polymerization monomer is polymerized, fix 30 ~ 50% scopes fine pitch, then by thermal station, compound system is heated, in another temperature range of 40 ~ 100 DEG C, employing wavelength is the ultraviolet light irradiation 5 ~ 100min of 254nm, and ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2, ultraviolet cationically polymerizable monomers is polymerized, fixes the coarse pitch of 50 ~ 70% scopes.
Step 3: by regulating the chiral compound substrate concentration in cholesteric liquid crystal, can prepare correspond to can reflect visible light district optical band or the N* phase liquid crystal hybrids system of reflect near IR district optical band, carry out ultraviolet light irradiation again, UV-light polymerisable monomer is polymerized, the ultraviolet light irradiation time is 5 ~ 100min, and ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2.
Further, described chipal compounds comprises the one in binaphthol, 4 '-(2-methyl butyl)-4-biphenyl cyanogen, Isosorbide and derivative thereof, and its helical twisting power reduces along with the increase of temperature.
Further, described ultraviolet free radical polymerization monomer is one or several in esters of acrylic acid, methyl acrylic ester, vinylbenzene base class, diacetyl base class, and active function groups quantity is 1 ~ 5.
Further, ultraviolet free radical photo-initiation is benzoin dimethylether IRG651.
Further, ultraviolet cationically polymerizable monomers is one or several in flexible chain redix or stiff chain redix, and active function groups quantity is 1 ~ 5.
Further, ultraviolet cation light initiator is two (4-tert.-butylbenzene) iodine hexafluorophosphates.
Further, the internal surface of liquid crystal cell is through planar orientation process, and planar orientation is treated to rubbing manipulation, Vacuum Coating method or chemical method.
Embodiment 1
(1) free yl polymerizating monomer C6M
(2) free radical photo-initiation IRG651
(3) cationic polymerization monomer EGDE
(4) cation light initiator BIH
(5) chipal compounds CD
The making of liquid crystal cell: get 3g polyvinyl alcohol (PVA) white solid particle and join in the deionized water of 97mL, magnetic agitation, is slowly heated to boiling, and namely it obtain concentration after all dissolving is the PVA solution of 3%.Sol evenning machine is used to carry out film to tin indium oxide (ITO) glass after cleaning up, coated conditions: initial velocity 300r/min, 9s, high speed 3000r/min, 30s, then to be placed in loft drier 90 DEG C to heat-treat the glass substrate being coated with PVA macromolecule membrane, 120 minutes time.After drying completes, with flannelette, 3 rubbings are carried out to the one side being coated with PVA oriented layer, avoid firmly excessive as far as possible.Above-mentioned two panels vitreous coating is had the substrate in combination of PVA, separation pad thickness is 20 μm, makes liquid crystal cell with glue sealing.
A) mass ratio: ultraviolet free radical polymerization monomer C6M/ ultraviolet free radical photo-initiation IRG651/ ultraviolet cationically polymerizable monomers EGDE/ ultraviolet cation light initiator BIH/ nematic liquid crystal SLC-1717/ chipal compounds CD.
Mixture system: be circulated into by sample 1 in the liquid crystal cell after carrying out surface treatment, 15 DEG C time, be 365nm with wavelength, ultraviolet ray intensity is 2mW/cm
2irradiation 10 minutes, is then heated to 60 DEG C by sample thermal station, is 254nm with wavelength, and ultraviolet light intensity is 2mW/cm
2each irradiation 10,20,30 minutes, makes polymerisable monomer curing cross-linked form network, namely obtains wide band photomasking film material after having irradiated.The position at wide wave reflection center can be changed by the content changing chipal compounds CD.
The instrument used in above-mentioned test process is ultraviolet-visible-near infrared spectrometer (JascoV-570).Sample is all be 15 DEG C in temperature, and liquid crystal molecule is the transmitted light spectrogram tested under the condition of planar texture, as can be seen from Figure 1, other condition is identical, the ultraviolet light irradiation time of 60 DEG C is different, and the wide difference of reflection wave, maximum reflection ripple is wide can reach 550nm (curve 4).
Embodiment 2
(1) free yl polymerizating monomer BDDA
(2) free radical photo-initiation IRG651
(3) cationic polymerization monomer EP-21
(4) cation light initiator BIH
(5) chipal compounds CD
B) mass ratio: ultraviolet free radical polymerization monomer BDDA/ ultraviolet free radical photo-initiation IRG651/ ultraviolet cationically polymerizable monomers EP-21/ ultraviolet cation light initiator BIH/ nematic liquid crystal SLC-1717/ chipal compounds CD.
Mixture system: be circulated into by sample 2 in the liquid crystal cell after carrying out surface treatment, 15 DEG C time, is 365nm with wavelength, ultraviolet ray intensity is respectively 2,4,6mW/cm
2each 10 minutes of irradiation, is then heated to 60 DEG C by sample thermal station, is then 254nm with wavelength, ultraviolet light intensity corresponds to 2 respectively, 4,6mW/cm
2irradiation 10 minutes again, makes polymerisable monomer curing cross-linked form network, namely obtains wide band photomasking film material after having irradiated.The position at wide wave reflection center can be changed by the content changing chipal compounds CD.
The instrument used in above-mentioned test process is ultraviolet-visible-near infrared spectrometer (JascoV-570).Sample is all be 15 DEG C in temperature, and liquid crystal molecule is the transmitted light spectrogram tested under the condition of planar texture, and as can be seen from Figure 2, when ultraviolet light irradiation intensity is different, reflection wave is wide different, and maximum reflection ripple is wide can reach 450nm (curve 8).
Embodiment 3:
(1) free yl polymerizating monomer IMA
(2) free radical photo-initiation IRG651
(3) cationic polymerization monomer PTTGE
(4) cation light initiator BIH
(5) chipal compounds C8
C) mass ratio: ultraviolet free radical polymerization monomer IMA/ ultraviolet free radical photo-initiation IRG651/ ultraviolet cationically polymerizable monomers PTTGE/ ultraviolet cation light initiator BIH/ nematic liquid crystal SLC-1717/ chipal compounds C8.
Mixture system: be circulated into by sample 3,4,5 in the liquid crystal cell after carrying out surface treatment, 15 DEG C time, be 365nm with wavelength, ultraviolet ray intensity is 6mW/cm
2irradiation 10 minutes, is then heated to 60 DEG C by sample thermal station, is 254nm with wavelength, and ultraviolet light intensity is 6mW/cm
2irradiation 10 minutes again, makes polymerisable monomer curing cross-linked form network, namely obtains wide band photomasking film material after having irradiated.
Embodiment 4
(1) free yl polymerizating monomer IMA
(2) free radical photo-initiation IRG651
(3) cationic polymerization monomer PTTGE
(4) cation light initiator BIH
(5) chipal compounds C8
D) mass ratio: ultraviolet free radical polymerization monomer IMA/ ultraviolet free radical photo-initiation IRG651/ ultraviolet cationically polymerizable monomers PTTGE/ ultraviolet cation light initiator BIH/ nematic liquid crystal SLC-1717/ chipal compounds C8
Mixture system: be circulated into by sample 6,7,8 in the liquid crystal cell after carrying out surface treatment, 15 DEG C time, be 365nm with wavelength, ultraviolet ray intensity is 6mW/cm
2irradiation 10 minutes, is then heated to 60 DEG C by sample thermal station, is 254nm with wavelength, and ultraviolet light intensity is 6mW/cm
2irradiation 10 minutes again, makes polymerisable monomer curing cross-linked form network, namely obtains wide band photomasking film material after having irradiated.
Esters of acrylic acid ultraviolet free radical polymerization monomer C6M in example can also replace by other esters of acrylic acid, methyl acrylic ester, vinylbenzene base class, diacetyl base class photopolymerizable monomer; Chipal compounds CD can also replace with 4 '-(2-methyl butyl)-4-biphenyl cyanogen, other Isosorbide and derivative thereof.
Claims (7)
1. ultraviolet step-by-step polymerization prepares a method for wide band photomasking film material, it is characterized in that, the method specifically comprises the following steps:
Step 1: nematic liquid crystal, chipal compounds, ultraviolet free radical polymerization monomer, ultraviolet free radical photo-initiation, ultraviolet cationically polymerizable monomers and ultraviolet cation light initiator are mixed according to certain mass ratio, wherein the weight percent of nematic liquid crystal is: 40 ~ 90%; The weight percent of chipal compounds is: 1 ~ 10%; The weight percent of ultraviolet free radical polymerization monomer is: 1 ~ 20%; The weight percent of ultraviolet free radical photo-initiation is: 0.1 ~ 10%; The weight percent of ultraviolet cationically polymerizable monomers is: 1 ~ 30%; 0.1 ~ 10% of the weight percent of ultraviolet cation light initiator, is heated to isotropy state by mixture, with oscillator vibrates repeatedly, mix, there is the transformation of isotropy state-cholesteryl phase in cooling, i.e. the cholesteric liquid crystal compound system of obtained mixture, lucifuge in operating process;
Step 2: the cholesteric liquid crystal compound system of step 1 mixture is circulated in advance in the liquid crystal cell of planar orientation process, the thickness of liquid crystal cell is 10 ~ 100 μm;
Step 3: by the liquid crystal cell of step 2 in the temperature range of 0 ~ 40 DEG C, employing wavelength is the ultraviolet light irradiation 5 ~ 100min of 365nm, and ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2, ultraviolet free radical polymerization monomer is polymerized, fix 30 ~ 50% scopes fine pitch, then by thermal station, compound system is heated, in another temperature range of 40 ~ 100 DEG C, employing wavelength is the ultraviolet light irradiation 5 ~ 100min of 254nm, and ultraviolet light irradiation degree is 0.1 ~ 100mW/cm
2, ultraviolet cationically polymerizable monomers is polymerized, fixes the coarse pitch of 50 ~ 70% scopes.
2. a kind of ultraviolet step-by-step polymerization according to claim 1 prepares the method for wide band photomasking film material, it is characterized in that: described chipal compounds comprises the one in binaphthol, 4 '-(2-methyl butyl)-4-biphenyl cyanogen, Isosorbide and derivative thereof, its helical twisting power reduces along with the increase of temperature, and the pitch of the cholesteric liquid crystal compound system of mixture increases along with the increase of temperature.
3. a kind of ultraviolet step-by-step polymerization according to claim 1 prepares the method for wide band photomasking film material; it is characterized in that: described ultraviolet free radical polymerization monomer is one or several in esters of acrylic acid, methyl acrylic ester, vinylbenzene base class, diacetyl base class, and active function groups quantity is 1 ~ 5.
4. a kind of ultraviolet step-by-step polymerization according to claim 1 prepares the method for wide band photomasking film material, it is characterized in that: described ultraviolet free radical photo-initiation is benzoin dimethylether IRG651.
5. a kind of ultraviolet step-by-step polymerization according to claim 1 prepares the method for wide band photomasking film material, it is characterized in that: described ultraviolet cationically polymerizable monomers is one or several in flexible chain redix or stiff chain redix, and active function groups quantity is 1 ~ 5.
6. a kind of ultraviolet step-by-step polymerization according to claim 1 prepares the method for wide band photomasking film material, it is characterized in that: described ultraviolet cation light initiator is two (4-tert.-butylbenzene) iodine hexafluorophosphate.
7. a kind of ultraviolet step-by-step polymerization according to claim 1 prepares the method for wide band photomasking film material, it is characterized in that: the internal surface of described liquid crystal cell is through planar orientation process, and planar orientation is treated to rubbing manipulation, Vacuum Coating method or chemical method.
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| CN108913159B (en) * | 2018-07-10 | 2021-02-12 | 北京科技大学 | Preparation method of visible light shielding film material |
| CN109031750A (en) * | 2018-08-22 | 2018-12-18 | 苏州美嘉写智能显示科技有限公司 | A kind of white light writing, reflection enhancement type liquid crystal board and preparation method thereof |
| CN109031750B (en) * | 2018-08-22 | 2022-06-10 | 苏州美嘉写智能显示科技有限公司 | White light handwriting and reflection enhanced liquid crystal writing board and preparation method thereof |
| CN112048279A (en) * | 2020-09-11 | 2020-12-08 | 为远材料科技(辽宁)有限责任公司 | Light-release adhesive, preparation method thereof and graphene transfer method |
| CN113391492A (en) * | 2021-06-23 | 2021-09-14 | 北京科技大学 | Near-infrared light shielding film material, preparation method and application |
| CN114656855A (en) * | 2022-03-15 | 2022-06-24 | 北京科技大学 | Preparation method and application of wide-wave-reflection flexible thin film material |
| CN115368599A (en) * | 2022-08-08 | 2022-11-22 | 北京科技大学 | Method for preparing temperature-adjustable broadband reflection liquid crystal film by temperature gradient method |
| CN115368599B (en) * | 2022-08-08 | 2023-09-05 | 北京科技大学 | Method for preparing temperature-adjustable broadband reflection liquid crystal film by temperature gradient method |
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