CN101148591A - Method for preparing liquid crystal thin film material with controllable reflection bandwidth - Google Patents
Method for preparing liquid crystal thin film material with controllable reflection bandwidth Download PDFInfo
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Abstract
The present invention is preparation process of liquid crystal film material with controllable reflecting bandwidth, and relates to preparation of material for light enhancing film and infrared shielding film for LCD. The liquid crystal film material is prepared through mixing nematic liquid crystal monomer capable of being light polymerized in 39.8-98.8 wt%, chiral compound in 1-60 wt% and photoinitiator in 0.2-5 wt% dissolved in solvent, and volatilizing the solvent to separate out cholest liquid crystal mixture; selecting powder of liquid crystal materials in different pitches based on required reflection bandwidth and reflection center and mixing; vacuum heating to cholest phase, pouring into preheated liquid crystal box in planar orientation, and ultraviolet radiating for 1-20 min for cross-linking reaction to prepare the liquid crystal film material. The liquid crystal film material has wide and adjustable reflection bandwidth.
Description
Technical field
The present invention relates to optically thin technology field of membrane materials, particularly a kind of liquid-crystal display optical reinforced film and infrared light shielded film material preparation method.
Background technology
Cholesteric liquid crystal is owing to its special spirane structure has the characteristic of selectivity Bragg reflection, and this particular optical performance makes cholesteric liquid crystal be applied in fields such as liquid-crystal display optical reinforced film, infrared photomasking film material widely.How effectively to increase the key point that reflection bandwidth is this type of technology.
Cholesteric liquid crystal is the nematic liquid crystal that has chirality, and two kinds of sources are generally arranged: the one, and itself has chiral radicals liquid crystal molecule, is the nematic phase that has spirane structure, i.e. cholesteric liquid crystal; Another kind of situation is to mix chipal compounds in nematic liquid crystal, and the structure of nematic liquid crystal is distorted, and obtains cholesteric liquid crystal.In a single-domain body, cholesteric liquid crystal molecule and screw shaft arranged vertical in the plane perpendicular to screw shaft, can be thought nematic liquid crystal; On the direction of screw shaft, the sensing generation successive of cholesteric liquid crystal molecule changes, during 360 ° of its rotations the length of screw shaft of process be called as pitch (representing) with P.The cholesteric liquid crystal reflected wavelength lambda of single pitch
o=Pn (wherein n is the average light specific refractory power of liquid crystal); Reflection spectrum bandwidth Δ λ=(n
e-n
o) P=Δ nP (Δ wherein
n=n
e-n
oBe degree of birefringence), be the poor of the respective wavelength that reaches maximum reflectivity 50% in the reflected light bands of a spectrum.In visible-range, the bandwidth of reflection spectrum is below 100nm usually.Under existence conditions, to effectively increase reflection bandwidth, can only set about from P, therefore method .Peter Palffy-Muhoray (the H Finkelmann that various realization pitch uneven distributions occurred, STKim, A Munoz, P Palffy-Muhoray et al, Advanced Materials 2001) etc. the people sets up the mesomorphic unit concentration gradient by the hot pressing diffusion of the mesomorphic unit between the vitreous state cholesteryl phase high molecule liquid crystal film with different pitch, the orientation back obtains the molecular spiral arrangement architecture and pitch gradient distributes, be easy to this structure is fixed up by quenching, weak point is: reflection wave is wide can not to be designed arbitrarily and control on demand with the reflection kernel wavelength.D.J.Broer (D.J.Broer, J.Lub, and G.N.Mol, Nature 1995) etc. the people use the composite system (comprise photopolymerization cholesteryl phase bifunctional acrylate, photopolymerization nematic phase simple function group acrylate, can absorb the dyestuff of UV-light etc.) of photopolymerization, be prepared into film.Because dyestuff is to the absorption of UV-light, film inside forms the Gradient distribution of ultraviolet ray intensity; Simultaneously, because photopolymerization cholesteryl phase bifunctional acrylate reacts the twice that probability is about photopolymerization nematic phase simple function group acrylate, in polymerization process, photopolymerization cholesteryl phase bifunctional acrylate is preferentially spread to the stronger side of film ultraviolet intensity.Thereby polymerization is finished and is formed pitch gradient in the rear film, and film can reflect whole visible light wave range (400-750nm) incident light.Because the degree that monomer spreads in liquid crystal is relevant with uv-radiation intensity, therefore the formed bandwidth of this method is very responsive to uv irradiating intensity, therefore in manufacturing processed, to use the monochromatic ray transmitter that polaroid is detected, in case reach required bandwidth, will improve uv-radiation intensity at once.Its equipment is complicated, the difficult control of technology.
Summary of the invention
The object of the invention is to provide a kind of preparation method with the controlled liquid-crystal film material of reflection bandwidth, can control reflection bandwidth and reflection kernel by the powder of selecting different pitch and the ratio of allocating between them, the liquid-crystal film material of preparation has semi-transparent more than half reflection characteristic, can cover whole visible light by suitable allotment respectively, near infrared, infrared band can be realized wide wave reflection, and it is complicated to overcome equipment, technology problem more rambunctious.
Concrete preparation technology of the present invention is:
1, the single pitch cholesteric liquid crystal that is mixed: photopolymerization nematic liquid crystal monomer, chipal compounds, light trigger are mixed according to different proportion of composing, photopolymerization nematic liquid crystal monomer is that 98.8-39.8wt%, chipal compounds are that 1-60wt%, light trigger are 0.2-5wt%, mixture is dissolved in the solvent mixes, under mixture fusing point or temperature below the second-order transition temperature and vacuum condition, solvent is all volatilized then, separate out the cholesteric liquid crystal mixture, mixture is in crystal form or vitreous state.
2, the cholesteryl phase solid state powder that is mixed and has different pitch: according to the wide and reflection kernel of expection reflection wave, selection has the powder of different pitch, 300-less than the 800nm wave band in, choose the cholesteric liquid crystal of a pitch every 100nm, in the 800-2500nm wave band, choose the cholesteric liquid crystal of a pitch every 300-400nm, then the cholesteric liquid crystal of the different pitch that will choose according to etc. the quality uniform mixing.
3, the powdered mixture that above-mentioned pitch is mixed is heated to cholesteryl phase under vacuum condition, guarantees that no air is residual in the mixture.Make it under mesomorphic state, inject the parallel-oriented liquid crystal cell of preheating then or be squeezed in double-layer films, after cholesteryl phase forms planar orientation, carry out the uv irradiation polymerization crosslinking, uv irradiation 1-20min, make the intermolecular generation crosslinking reaction of photopolymerizable monomer, ultraviolet wavelength is 365nm, irradiation dose 0.001-100mWcm
-2Nonlinear pitch gradient distribution is permanently fixed in the film like this, thereby obtain the liquid-crystal film material of wide band reflection, described reflected wavelength range can cover whole visible light respectively according to the pitch difference of the selected powder that is mixed, near infrared, or infrared band.
Photopolymerization nematic liquid crystal monomer of the present invention is esters of acrylic acid, methyl acrylic ester, vinylbenzene base class, diacetyl base class, and the quantity of active function groups is 1～5; Described chipal compounds is cholesterol class and non-cholesterol class; Described light trigger is selected any in dibenzoyl peroxide, dilauroyl peroxide, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), di-isopropyl peroxydicarbonate, the di-cyclohexylperoxy dicarbonate; The solvent that is used to dissolve mixed liquid crystal monomer, chipal compounds and light trigger is any of organic solvents such as acetone, ethanol, methylene dichloride, trichloromethane.
For guarantee to have the uneven distribution of pitch in as far as possible little microcell, the standby mixture with single pitch of the present invention must grind under crystal form or vitreous state, and being ground to diameter of particle is 1～20 μ m.
The liquid crystal compound of different pitch all is under crystal form or the vitreous state at mixture and mixes.In order to adjust pitch, can introduce other chirality or achirality small molecules liquid crystal in the moiety of cholesteric liquid crystal mixture.Do not spread when even in its concentration for the liquid crystal compound that guarantees to be mixed simultaneously by different pitch requirements, the uneven distribution of fixed pitch, must be will be mixed liquid crystal compound inject 5-300 μ m liquid crystal cell, its mesomorphic phase is carried out uv irradiating after being the state of planar texture immediately.
After guaranteeing that liquid crystal injects liquid crystal cell, more easily form planar texture within a short period of time, liquid crystal cell of the present invention should shift to an earlier date preheating, and preheating temperature is the uv irradiating temperature, can choose in the cholesteryl phase temperature range.
Temperature can be in arbitrary temp in the whole mesomorphic phase temperature range of mixture during uv irradiation polymerization crosslinking of the present invention, and do not carry out before liquid crystal between the powder of different pitch or chipal compounds molecule spread homogeneous as yet, make photo polymerization monomer be cross-linked into macromolecule network.
The moiety of powder of the present invention is except that above-mentioned several compositions: photo-polymerizable liquid crystal monomer, chipal compounds, the light trigger, can also introduce other chirality or achirality small molecules liquid crystal to adjust pitch, or according to selected composition, technology and actual demand, whether decision adds other components such as stopper, dyestuff.
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A) some can be used for the photo-polymerizable liquid crystal monomer among the present invention, but are not limited to these materials.
(20)
ZLI-4572
(21)
Cholesterol
(22)
C15
(23)
CB15
(24)
S811 and R811
B) can be used for chipal compounds among the present invention, but be not limited to these materials.
Light trigger Irgacure 651
C) can be used for a kind of light trigger among the present invention, but be not limited to these materials.
The present invention can realize the wide ripple liquid-crystal film material of semi-transparent more than half reflection characteristics, and the preparation method of this kind reflective liquid crystal thin-film material and previous methods relatively have the following advantages:
1, material system used in the present invention is more simple, and material source is extensive
2, the present invention is not very sensitive to UV intensity, directly adopt less or big light intensity all can, thereby preparation equipment is simple, control easily.
3, the present invention can obtain the wide and reflection kernel of predefined reflection wave by the powder of selecting required different pitch and the ratio of allocating them.
Description of drawings
Fig. 1 is cholesteric liquid crystal molecular spiral arrangement architecture and nonlinear pitch gradient distribution plan among the embodiment among the present invention.
Fig. 2 is the transmitted light spectrogram of the wide wave reflection liquid crystal polarizer of the embodiment of the invention 1.
1,2,3-95 ℃, uv irradiation intensity is 8.4mWcm
-2Condition under realize the transmitted spectrum of the liquid crystal compound of the single pitch of the 400-750nm required blended of wide waveband wave reflection, reflection kernel is respectively: 400nm, 550nm, 756nm;
A-95 ℃, uv irradiation intensity is 8.4mWcm
-2Condition under realize the transmitted spectrum of the mixed liquid crystal compound of different pitch of 400-800nm wide waveband wave reflection.
Fig. 3 is the transmitted light spectrogram of the wide wave reflection liquid crystal polarizer of the embodiment of the invention 2.
4,5,6-95 ℃, uv irradiation intensity is 8.4mWcm
-2Condition under realize the transmitted spectrum of the liquid crystal compound of the single pitch of the 1100-2500nm required blended of wide waveband wave reflection, reflection kernel is respectively: 1162nm, 1822nm, 2510nm;
B-95 ℃, uv irradiation intensity is 8.4mWcm
-2Condition under realize the transmitted spectrum of the mixed liquid crystal compound of different pitch of 1100-2500nm wide waveband wave reflection.
Embodiment
The invention will be further described for following examples, and the present invention not only is defined in this embodiment.
Embodiment 1
Use photopolymerizable nematic liquid crystal monomer C6M, its molecular formula is shown in photo-polymerizable liquid crystal monomer (4), chipal compounds is the ZLI-4572 of Merck company, its molecular formula is shown in chipal compounds (20), light trigger is the Irgacure 651 of TCI company, and its molecular formula is dissolved in the acetone by different ratios shown in light trigger (25), wherein, light trigger Irgacure 651 accounts for 0.5% of gross weight; 1,2, No. 3 corresponding component C 6M/ZLI4572 of curve weight percents are respectively 87.8/12.2,91.0/9.0,93.7/12.2.Ultrasonic concussion mixes mixture, under the lucifuge condition, vacuumizes solvent flashing, and mixture is separated out, and is solid state, and it is standby less than the powder of 3 μ m to grind into particle diameter.Desire prepares that reflection wave is wide to be the film of 400-800nm, and configurable reflection kernel wavelength is respectively the powder with single pitch of 756nm, 550nm, 400nm.Be the powder that 1: 1: 1 mixed reflection centre wavelength is respectively 756nm, 550nm, 400nm by weight proportion, mixed mixture is vacuumized 5min,, prevent the appearance of polymerization rear film inside aperture, influence Film Optics character to drain air.Utilize the phase transition temperature of three kinds of single pitch powder of dsc measurement to be respectively 81.2 ℃-109.8 ℃, 81 ℃-108.1 ℃ and 82.3 ℃-106.4 ℃, the mixture heating up to 95 of three kinds of therefore that the reflection kernel wavelength is different powder ℃, this moment, three kinds of powder all were liquid crystal state, and good fluidity is easy to form planar texture preferably.For reducing experimental error, shorten the diffusion time before injecting liquid crystal cell between different pitch powder, liquid crystal cell also must be preheated to 95 ℃ in advance.At last, the mixture of three kinds of powder is injected planar orientation, thickness is the liquid crystal cell of 40 μ m, behind the planar texture that just is in vitreous state, uses 365nm intensity to be 8.4mW/cm immediately
-2The about 5min of UV-irradiation, irradiation temperature is identical with the liquid crystal filling temperature, along with the vertical plane differently-oriented directivity on the inhomogeneous Gradient distribution of non-linear pitch be fixed, like this, the liquid-crystal film material of realizing wide wave reflection is made, the wide 400-800nm that reaches of reflection wave, light transmission rate approximate 50%.The A curve is its transmitted light spectrogram among Fig. 2.
Embodiment 2
Use photopolymerizable nematic liquid crystal monomer C6M, its molecular formula is shown in photo-polymerizable liquid crystal monomer (4), chipal compounds is the ZLI-4572 of Merck company, its molecular formula is shown in chipal compounds (20), light trigger is the Irgacure 651 of TCI company, its molecular formula is shown in light trigger (25), be dissolved in the acetone by different ratios, wherein, the corresponding component C 6M/ZLI4572 of 0.5%, 4,5, No. 6 curve weight percent that light trigger Irgacure 651 accounts for gross weight is respectively 96.6/3.4,97.4/2.6,98.1/1.9.Ultrasonic concussion mixes mixture, under the lucifuge condition, vacuumizes solvent flashing, and mixture is separated out, and is solid state, and it is standby less than the powder of 3 μ m to grind into particle diameter.Desire prepares that reflection wave is wide to be the film of 1100-2500nm, and configurable reflection kernel wavelength is respectively the powder with single pitch of 2500nm, 1816nm, 1160nm.Be the powder that 1: 1: 1 mixed reflection centre wavelength is respectively 2500nm, 1816nm and 1160nm by weight proportion, mixed mixture is vacuumized 5min,, prevent the appearance of polymerization rear film inside aperture, influence Film Optics character to drain air.Utilize the phase transition temperature of three kinds of single pitch powder of dsc measurement to be respectively 82.7 ℃-114.2 ℃, 82.3 ℃-113.6 ℃ and 81.6 ℃-111.7 ℃, the mixture heating up to 95 of three kinds of therefore that the reflection kernel wavelength is different powder ℃, this moment, three kinds of powder all were liquid crystal state, and good fluidity is easy to form planar texture preferably.For reducing experimental error, shorten the diffusion time before injecting liquid crystal cell between different pitch powder, liquid crystal cell also must be preheated to 95 ℃ in advance.At last, the mixture of three kinds of powder is injected planar orientation, thickness is the liquid crystal cell of 100 μ m, behind the planar texture that just is in vitreous state, uses 365nm intensity to be 8.4mW/cm immediately
-2The about 5min of UV-irradiation, irradiation temperature is identical with the liquid crystal filling temperature, along with the vertical plane differently-oriented directivity on the inhomogeneous Gradient distribution of non-linear pitch be fixed, like this, the liquid-crystal film material of realizing wide wave reflection is made, the wide 1100-2500nm that reaches of reflection wave, light transmission rate approximate 50%.The B curve is its transmitted light spectrogram among Fig. 3.
Claims (7)
1. the preparation method of the controlled liquid-crystal film material of a reflection bandwidth is characterized in that step of preparation process is:
A) the single pitch cholesteric liquid crystal that is mixed: the photopolymerization nematic liquid crystal monomer of 98.8-39.8wt%, the chipal compounds of 1-60wt%, the light trigger uniform mixing of 0.2-5wt% are dissolved in the solvent, under cholesteric liquid crystal mixture fusing point or temperature below the second-order transition temperature and vacuum condition, solvent is all volatilized then, separate out the cholesteric liquid crystal mixture, the cholesteric liquid crystal mixture is in crystal form or vitreous state;
B) the cholesteryl phase solid state powder that is mixed and has different pitch: according to the wide and reflection kernel of expection reflection wave, selection has the powder of different pitch, 300-less than the 800nm wave band in, choose the cholesteric liquid crystal of a pitch every 100nm, in the 800-2500nm wave band, choose the cholesteric liquid crystal of a pitch every 300-400nm, then the cholesteric liquid crystal of the different pitch that will choose according to etc. the quality uniform mixing;
C) the cholesteric liquid crystal powder that will have different pitch by etc. the powdered mixture that is mixed of quality under vacuum condition, be heated to cholesteryl phase; guaranteeing does not have air in the mixture; make it under mesomorphic state, inject the parallel-oriented liquid crystal cell of preheating then or be squeezed in double-layer films; after cholesteryl phase forms planar orientation; carry out the uv irradiation polymerization crosslinking; uv irradiation 1-20min, ultraviolet wavelength are 365nm, irradiation dose 0.001-100mWcm
-2
2. method according to claim 1 is characterized in that, described photopolymerization nematic liquid crystal monomer be in esters of acrylic acid, methyl acrylic ester, vinylbenzene base class, the diacetyl base class any, the quantity of active function groups is 1～5; Described chipal compounds is cholesterol class and non-cholesterol class; Described light trigger is selected any in dibenzoyl peroxide, dilauroyl peroxide, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), di-isopropyl peroxydicarbonate, the di-cyclohexylperoxy dicarbonate; The solvent that is used for dissolving mixed liquid crystal monomer, chipal compounds and light trigger is any of acetone, ethanol, methylene dichloride, trichloromethane organic solvent.
3. method according to claim 1 is characterized in that, the cholesteric liquid crystal mixture of single pitch is ground under crystal form or vitreous state, and grinding the back particle diameter is 1-20 μ m.
4. method according to claim 1 is characterized in that, the moiety of described cholesteric liquid crystal mixture can be introduced other chirality or achirality small molecules liquid crystal to adjust pitch.
5. according to claim 1 or 4 described methods, it is characterized in that the cholesteric liquid crystal of the different pitch of choosing all is under crystal form or the vitreous state at mixture and mixes.
6. method according to claim 1, it is characterized in that, the parallel-oriented liquid crystal cell of described injection preheating, it is the liquid crystal cell that the liquid crystal compound that will be mixed injects 5-300 μ m, the internal surface of liquid crystal cell or film carries out parallel-oriented, preheating temperature is the uv irradiating temperature, chooses in the cholesteryl phase temperature range.
7. method according to claim 1, it is characterized in that, temperature is in the interior arbitrary temp of mesomorphic phase temperature range of mixture during the uv irradiation polymerization crosslinking, and do not carry out before liquid crystal between the powder of different pitch or chipal compounds molecule spread homogeneous as yet, make photo polymerization monomer be cross-linked into macromolecule network.
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