CN104531164B - High molecular reinforced negative cholesteric phase mixed liquid crystal material and application method thereof - Google Patents
High molecular reinforced negative cholesteric phase mixed liquid crystal material and application method thereof Download PDFInfo
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Abstract
The invention relates to a high molecular reinforced negative cholesteric phase mixed liquid crystal material, which comprises, by mass, 90-98% of negative dielectric anisotropy nematic liquid crystal, 2-5% of a chiral additive, 2-8% of a polymerizable end group containing high molecular material prepolymer or monomer, a photoinitiator with an adding amount of 500-2000ppm, and cetyl trimethyl ammonium bromide with an adding amount of 300-800ppm. Through improvement of the formula, based on bistable reality, the high molecular reinforced negative cholesteric phase mixed liquid crystal material has lower conversion frequency, higher mist state shielding property and higher on-state penetration.
Description
Technical field
The present invention relates to lcd technology, particularly to bi-stable liquid crystal material and its application process.
Background technology
Liquid crystal display (lcd), as an important application of this special material of liquid crystal, finds soon from liquid crystal characteristic
Just obtain the extensive concern of people always.Recent decades, particularly the developing rapidly and people of information technology in recent ten years
Continuous pursuit to information display methods, liquid crystal display has obtained development the swiftest and the most violent.Today, liquid crystal display is just with colourful
Form be illustrated in face of people, its many products make it just become the pursuit of fashion, Yi Jishang due to its excellent characteristic
The available commodity of handss are processed in.
Liquid crystal display experienced very long road for development with the discovery of liquid crystal.Austrian botanist in 1888
Friedrich reinitzer is found that the first liquid crystal material benzoic acid cholesterol (cholesteryl benzoate).
Manguin has invented rubbing within 1917, in order to make single domain liquid crystal and research optical anisotropy.E.bose in 1909
Establish and collect together (swarm) theory, and obtain the experiment of l.s.ormstein and f.zernike et al. and support (1918), after
It is discussed as statistical fluctuation through de gennes.G.w.oseen and h.zocher1933 foundes continuum theory, and obtains
F.c.frank perfect (1958).M.born (1916) and k.lichtennecker (nineteen twenty-six) finds and have studied liquid crystal
Dielectric anisotropy.1932, nematic phase was divided into positive and negative property two big class by w.kast accordingly.Nineteen twenty-seven,
V.freedericksz and v.zolinao finds that nematic liquid crystal, under electric field (or magnetic field) effect, deforms upon and there is electricity
Pressure threshold value (freederichsz transformation).The making that this is found to be liquid crystal display provides foundation.
Nineteen sixty-eight U.S. rca company r.williams finds that nematic liquid crystal forms striped farmland under electric field action, and has
Light scattering phenomenon.G.h.heilmeir is with it will developing into dynamic scattering display pattern, and makes first liquid crystal in the world
Display (lcd).Nineteen sixty-eight U.S. heilmeir et al. also proposed guest-host effect (gh) pattern.Xerox company carries within 1969
Go out ch-n phase change memory pattern.M.f.schiekel proposes electrically conerolled birefringence (ecb) pattern within 1971, and t.l.fergason etc. carries
Go out twisted nematic (twisted nematic:tn) pattern, n.clark in 1980 etc. proposes ferroelectric liquid crystals pattern (flc),
1983～1985 years t.scheffer et al. successively propose super-twist nematic (super twisred nematic:stn) pattern
And p.brody is adopted again in active matrix (active matrix:am) mode that 1972 propose.1986
White and black displays technology is realized in nagata proposition bilayer box (dstn)；Useful stretching polymeric membrane realizes white and black displays again afterwards
Technology (fstn).After 1996, the reflective tn (rtn) using single polaroid and reflective stn (rstn) mould are proposed again
Formula.
According to the similarities and differences of control device and principle, dimming glass can be by automatically controlled, temperature control, light-operated, voltage-controlled etc. various sides
Formula realizes the switching of the transparent of glass and opaque state.The dimming glass that wherein temperature control, light-operated and voltage-controlled fabrication techniques go out is subject to
The Yi Su impact of environment is very big, is not the dimming glass of the Autonomous Control in complete meaning.
Known Korean's invention can suspended particles class dimming glass be a kind of tune of use electrochromism fabrication techniques
Light glass.This kind of glass is between the layer glass of dimming glass, adjusts the saturating of light by controlling suspended particles quantity
Penetrate and scatter degree, the shortcoming of this dimming glass is that cost is very high, and in order to prevent particle reveal, to operation and use ring
The requirement in border is very high.In addition to using electrochromism fabrication techniques dimming glass, also can complete by mechanical means to dim
(such as Chinese utility model patent zl200320116206.8).This mechanical means are mainly two of the laminated glass in hollow
Two spools are placed at end, are wrapped with multiple colorful films to realize above spool, when needing shading, by a kind of thin film rotation of color
Out shading, and when needing printing opacity, it is possible to use control the motor of spool that the colorful film of shading is accepted, this machine
The maximum shortcoming of tool mode is to need manual operation, structure bulky, and poor reliability, and service life is short.
In addition, a kind of known electroluminescent dimming glass is to be realized using PDLC (pdlc) technology.This skill
Art by University of Kent joseph w doctor doane leader group in 1984 invent, United States Patent (USP) us4688900.This
Technology uses water-fast polymer monomer, such as epoxy resin and firming agent, mix with liquid crystal and formed one transparent
Solution.When solidification occurs, because dissolubility reduces, liquid crystal particle can separate out automatically, and is suspended in macromolecule phase.This work
Skill includes (1) and prepares liquid crystal, the solution of epoxy resin and firming agent, and (2) are before curing, solution combined conductive in two-layer by this
Between thin film, (3) are heating and curing the thin film being combined.Pdlc technique can only produce eurymeric product.Eurymeric pdlc product is not
It is milky during energising, after energising, be changed into transparent.
Pdlc technology has good switch state photoelectricity effect, however it is necessary that lasting power supply is maintaining pellucidity.Separately
Outer have obvious viewing angle problem due to the defect of technology itself, although being changed into clear state, from side-looking angular direction after being energized
Observe, still show a certain degree of mist state.
Invent a kind of macromolecule enhancing negativity cholesteric liquid crystal that is based on for this United States Patent (USP) us20090290078 to show.
But this driving needs the up to driving frequency of 100khz to be unfavorable for large-scale promotion.
Content of the invention
It is an object of the invention to provide a kind of macromolecule strengthens the mixed liquid crystal material of negativity cholesteric liquid crystal display,
Solve the technical problem that in prior art, visual angle is bad and driving frequency is too high.
The macromolecule providing for solving above-mentioned technical problem in the present invention strengthens negativity cholesteric phase mixed liquid crystal material bag
Include in mass ratio 90～98% negative dielectric anisotropic nematic liquid crystal, 2～5% chiral additiveses, 2～8%
Macromolecular material prepolymer containing polymerisable terminal groups or light trigger that monomer, addition are 500～2000ppm and interpolation
Measure the cetyl trimethylammonium bromide for 300～800ppm.
Described negative dielectric anisotropic nematic liquid crystal includes the first compound of following structural formula:
Wherein r1、r2Independently be 2 to 9 carbon atoms alkyl or alkoxyl.
Described negative dielectric anisotropic nematic liquid crystal includes the second compound of following structural formula:
Wherein r3、r4Independently be 2 to 9 carbon atoms alkyl or alkoxyl, m=0 or 1, n=0 or 1,WithDifference, independently beOr
Described negative dielectric anisotropic nematic liquid crystal includes the 3rd compound of following structural formula:
Wherein r7、r8Independently be 2 to 9 carbon atoms alkyl or alkoxyl.
Described negative dielectric anisotropic nematic liquid crystal includes the 4th compound of following structural formula:
Wherein r9、r10Independently be 2 to 9 carbon atoms alkyl or alkoxyl, p=0 or 1, q=0 or 1,WithDifference, independently beOr
First compound, second compound, the 3rd compound and in described negative dielectric anisotropic nematic liquid crystal
Between four compounds, ratio in mass ratio is 5～30% the first compound；10～40% second compound；10～30%
The 3rd compound and 20～40% the 4th compound.
Described chiral additiveses are:
The r/s811 of structural formula；Or
PersonStructural formula
r/s1011.
The described macromolecular material prepolymer containing polymerisable terminal groups or monomer are:
The divinylbenzene of structural formula.
Described light trigger is:
The irgacure 819 of structural formula.
The application process that this macromolecule strengthens negativity cholesteric phase mixed liquid crystal material comprises the following steps:
A. with electronic balance in proportion precise negative dielectric anisotropic nematic liquid crystal, chiral additiveses, containing can
The macromolecular material prepolymer of polymerization end groups or monomer, light trigger and cetyl trimethylammonium bromide, and mix；
B. by the way of shading stirring, above-mentioned material is stirred 100～130 minutes at normal temperatures；
C. the mixed liquid crystal material after the stirring of step b is poured in liquid crystal cell；
D. after irrigation crystal mouth dispensing, with the solidification of uv light irradiation.
The present invention by the improvement of formula so as to tool, on the basis of bistable state reality, has lower conversion frequency,
Higher mist state shielding and the ON state penetration of Geng Gao.
Brief description
Fig. 1 is the schematic diagram of practical application of the present invention.
In figure labelling: 1 liquid crystal and separaant；2 frames；3 ito glass.
Specific embodiment
The specific embodiment of the detailed description below present invention.
Macromolecule of the present invention strengthens negative Jie that negativity cholesteric phase mixed liquid crystal material includes in mass ratio 90～98%
Electrical anisotropy nematic liquid crystal, 2～5% chiral additiveses, 2～8% the macromolecular material containing polymerisable terminal groups pre-
Polymers or light trigger that monomer, addition are 500～2000ppm and the cetyl three that addition is 300～800ppm
Methyl bromide ammonium.The adjustment by material mixture ratio for the present invention, in order to improve the intersolubility of liquid crystal, the masking mist degree of state, ON state
Penetration and reduction driving frequency.
More preferred mixed liquid crystal material mixture ratio (in mass ratio) in the present invention be 93～95% negative dielectric respectively to different
Property nematic liquid crystal, 2～3% chiral additiveses, 4～6% macromolecular material prepolymer containing polymerisable terminal groups or list
Body, addition are the light trigger of 800～1200ppm and cetyl trimethyl bromination that addition is 450～550ppm
Ammonium.
The present invention specific material selection scheme is as follows: described negative dielectric anisotropic nematic liquid crystal includes following structure
First compound of formula:
It is labeled as；
Wherein r1、r2Independently be 2 to 9 carbon atoms alkyl or alkoxyl, adopt structure above in the present invention
Compound be used for reducing driving frequency.
And the preferred version of the first compound is the combination of one or more of following structural formula:
It is labeled as 1；
It is labeled as 2；
It is labeled as 3；
It is labeled as 4.
Described negative dielectric anisotropic nematic liquid crystal includes the second compound of following structural formula:
It is labeled as,
Wherein r3、r4Independently be 2 to 9 carbon atoms alkyl or alkoxyl, m=0 or 1, n=0 or 1,WithDifference, independently beOrUsing structure above
Compound, for improving the transmitance of ON state.
The combination of one or more of second compound preferably following structural formula in the present invention:
It is labeled as 1；
It is labeled as 2；
It is labeled as 3；
It is labeled as 4；
It is labeled as 5；
It is labeled as 6；
It is labeled as 7；
It is labeled as 8；
It is labeled as 9；
It is labeled as 10；
It is labeled as 11；
It is labeled as 12.
Negative dielectric anisotropic nematic liquid crystal of the present invention includes the 3rd compound of following structural formula:It is labeled as；
Wherein r7、r8Independently be 2 to 9 carbon atoms alkyl or alkoxyl, using the chemical combination of structure above
Thing, for providing the mist degree of masking state.
The combination of one or more of the 3rd compound preferably following structural formula in the present invention:
It is labeled as 1；
It is labeled as 2；
It is labeled as 3；
It is labeled as 4.
Negative dielectric anisotropic nematic liquid crystal of the present invention includes the 4th compound of following structural formula:It is labeled as；
Wherein r9、r10Independently be 2 to 9 carbon atoms alkyl or alkoxyl, p=0 or 1, q=0 or 1,WithDifference, independently beOrTo mix for improving this
The intersolubility (preventing low temperature crystallize) of fit system, is simultaneously also beneficial to improve the penetration of ON state.
The combination of one or more of the 4th compound preferably following structural formula in the present invention:
It is labeled as 1；
It is labeled as 2；
It is labeled as 3；
It is labeled as 4；
It is labeled as 5；
It is labeled as 6；
It is labeled as 7；
It is labeled as 8；
It is labeled as 9；
It is labeled as 10；
It is labeled as 11；
It is labeled as 12.
First compound, second compound, the 3rd chemical combination in heretofore described negative dielectric anisotropic nematic liquid crystal
Between thing and the 4th compound, ratio in mass ratio is 5～30% the first compound；10～40% second compound；
10～30% the 3rd compound and 20～40% the 4th compound.Wherein preferably scheme is described negative dielectric respectively to different
Ratio in mass ratio between first compound, second compound, the 3rd compound and the 4th compound in property nematic liquid crystal
First compound for 10～20% for the example；20～40% second compound；15～25% the 3rd compound and 30～
40% the 4th compound.
Heretofore described chiral additiveses are:
The r/s811 of structural formula；Or
PersonThe r/s1011 of structural formula.
The described macromolecular material prepolymer containing polymerisable terminal groups or monomer are:
The divinylbenzene of structural formula.
Described light trigger is:
The irgacure 819 of structural formula.
In the present invention, example in actual cooperation for the mixed liquid crystal material is as follows:
Negative dielectric anisotropic nematic liquid crystal proportioning example one, is labeled as scheme a1:
| Component | Percentage by weight (%) | Performance parameter | Parameter value |
| ⅰ-1 | 5 | cp | 89 |
| ⅰ-3 | 5 | δε | -7.7 |
| ⅱ-2 | 12 | δn | 0.158 |
| ⅱ-7 | 13 | ||
| ⅱ-12 | 5 | ||
| ⅲ-1 | 7 | ||
| ⅲ-4 | 8 | ||
| ⅳ-4 | 20 | ||
| ⅳ-6 | 10 | ||
| ⅳ-9 | 5 |
The proportioning example two of negative dielectric anisotropic nematic liquid crystal, is labeled as scheme a2:
| Component | Percentage by weight (%) | Performance parameter | Parameter value |
| ⅰ-2 | 10 | cp | 91 |
| ⅰ-4 | 10 | δε | -8.6 |
| ⅱ-3 | 12 | δn | 0.163 |
| ⅱ-6 | 13 | ||
| ⅱ-11 | 10 | ||
| ⅲ-1 | 7 | ||
| ⅲ-3 | 8 | ||
| ⅳ-3 | 15 | ||
| ⅳ-5 | 6 | ||
| ⅳ-6 | 6 | ||
| ⅳ-10 | 3 |
Mixed liquid crystal proportioning and liquid crystal applications scheme 1:
| Component | Percentage by weight | Uv intensity | 100mw/cm2 |
| a1 | 93% | Uv irradiation time | 10min |
| r1011 | 2% | Through state drive condition | 50v, 8khz |
| c | 5% | Masking state drive condition | 50v, 50hz |
| d | 500ppm | ON state transmitance | 91% |
| e | 300ppm | ON state mist degree | 3% |
| Masking state transmitance | 5% | ||
| Masking state mist degree | 87% |
Mixed liquid crystal proportioning and liquid crystal applications scheme 2:
| Component | Percentage by weight | Uv intensity | 80mw/cm2 |
| a2 | 92.5% | Uv irradiation time | 12min |
| s011 | 3% | Through state drive condition | 50v, 1khz |
| c | 4.5% | Masking state drive condition | 50v, 50hz |
| d | 600ppm | ON state transmitance | 93% |
| e | 400ppm | ON state mist degree | 3.5% |
| Masking state transmitance | 4% | ||
| Masking state mist degree | 85% |
The application process that macromolecule of the present invention strengthens negativity cholesteric phase mixed liquid crystal material comprises the following steps:
A. with electronic balance in proportion precise negative dielectric anisotropic nematic liquid crystal, chiral additiveses, containing can
The macromolecular material prepolymer of polymerization end groups or monomer, light trigger and cetyl trimethylammonium bromide, and mix；
B. by the way of shading stirring, above-mentioned material is stirred 100～130 minutes at normal temperatures；
C. the mixed liquid crystal material after the stirring of step b is poured into (see Fig. 1) in liquid crystal cell；
D. after irrigation crystal mouth dispensing, with the solidification of uv light irradiation.
Mixing time wherein in step b be preferably 115～125 minutes, in step d the illumination index of uv lamp be 10～
160mw/cm2, light application time is 1～15 minute.
Above content is to further describe it is impossible to assert with reference to specific preferred implementation is made for the present invention
Being embodied as of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of present inventive concept, some simple deduction or replace can also be made, all should be considered as belonging to the present invention's
Protection domain.
Claims (16)
1. a kind of macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: this mixed liquid crystal material is included by matter
Amount proportioning be 90～98% negative dielectric anisotropic nematic liquid crystal, 2～5% chiral additiveses, 2～8% containing can
The macromolecular material prepolymer of polymerization end groups or the light trigger that monomer, addition are 500～2000ppm and addition are
The cetyl trimethylammonium bromide of 300～800ppm, described negative dielectric anisotropic nematic liquid crystal includes following structural formula
The first compound:
Wherein r1、r2Independently be 2 to 9 carbon atoms alkyl or alkoxyl.
2. according to claim 1 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: this mixed liquid crystal
The proportioning of material in mass ratio be 93～95% negative dielectric anisotropic nematic liquid crystal, 2～3% chiral additiveses, 4～
The 6% macromolecular material prepolymer containing polymerisable terminal groups or light trigger that monomer, addition are 800～1200ppm with
And the cetyl trimethylammonium bromide that addition is 450～550ppm.
3. according to claim 1 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described first change
Compound includes the combination of one or more of following structural formula:
4. according to claim 1 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described negative dielectric
Anisotropy nematic liquid crystal includes the second compound of following structural formula:
Wherein r3、r4Independently be 2 to 9 carbon atoms alkyl or alkoxyl, m=0 or 1, n=0 or 1,Difference, independently be
5. according to claim 4 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described second change
Compound includes the combination of one or more of following structural formula:
6. according to claim 4 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described negative dielectric
Anisotropy nematic liquid crystal includes the 3rd compound of following structural formula:
Wherein r7、r8Independently be 2 to 9 carbon atoms alkyl or alkoxyl.
7. according to claim 6 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described 3rd change
Compound includes the combination of one or more of following structural formula:
8. according to claim 6 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described negative dielectric
Anisotropy nematic liquid crystal includes the 4th compound of following structural formula:
Wherein r9、r10Independently be 2 to 9 carbon atoms alkyl or alkoxyl, p=0 or 1, q=0 or 1,Difference, independently be
9. according to claim 8 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described 4th change
Compound includes the combination of one or more of following structural formula:
10. according to claim 8 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described negative Jie
Matter is pressed between first compound, second compound, the 3rd compound and the 4th compound in electrical anisotropy nematic liquid crystal
The ratio of amount ratio is 5～30% the first compound；10～40% second compound；10～30% the 3rd compound and
20～40% the 4th compound.
11. according to claim 8 macromolecule strengthen negativity cholesteric phase mixed liquid crystal material it is characterised in that: described negative Jie
Matter is pressed between first compound, second compound, the 3rd compound and the 4th compound in electrical anisotropy nematic liquid crystal
The ratio of amount ratio is 10～20% the first compound；20～40% second compound；15～25% the 3rd compound with
And 30～40% the 4th compound.
12. macromolecules according to any one of claim 1 to 11 strengthen negativity cholesteric phase mixed liquid crystal material, and its feature exists
In: described chiral additiveses are:
The r/s811 of structural formula；
OrThe r/s1011 of structural formula.
13. macromolecules according to any one of claim 1 to 11 strengthen negativity cholesteric phase mixed liquid crystal material, and its feature exists
In: the described macromolecular material prepolymer containing polymerisable terminal groups or monomer are:
The divinylbenzene of structural formula.
14. macromolecules according to any one of claim 1 to 11 strengthen negativity cholesteric phase mixed liquid crystal material, and its feature exists
In: described light trigger is:
The irgacure 819 of structural formula.
A kind of 15. macromolecules as any one of claim 1 to 14 strengthen the application of negativity cholesteric phase mixed liquid crystal material
Method it is characterised in that: the method comprises the following steps:
A. with electronic balance in proportion precise negative dielectric anisotropic nematic liquid crystal, chiral additiveses, contain polymerizable
The macromolecular material prepolymer of end group or monomer, light trigger and cetyl trimethylammonium bromide, and mix；
B. by the way of shading stirring, above-mentioned material is stirred 100～130 minutes at normal temperatures；
C. the mixed liquid crystal material after the stirring of step b is poured in liquid crystal cell；
D. after irrigation crystal mouth dispensing, with the solidification of uv light irradiation.
16. application processes according to claim 15 it is characterised in that: the mixing time in step b be 115～125 points
Clock, in step d, the illumination index of uv lamp is 10～160mw/cm2, light application time is 1～15 minute.
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| KR102041819B1 (en) * | 2015-08-28 | 2019-11-07 | 주식회사 엘지화학 | Normally transparent liquid crystal device |
| CN105860995B (en) * | 2016-04-19 | 2019-01-22 | 京东方科技集团股份有限公司 | A kind of composition, liquid crystal display device and preparation method thereof |
| JP7419537B2 (en) * | 2019-12-24 | 2024-01-22 | 北京八億時空液晶科技股▲ふん▼有限公司 | Low viscosity, fast response liquid crystal compositions and applications in liquid crystal displays |
| CN113736474A (en) * | 2020-05-29 | 2021-12-03 | 江苏集萃智能液晶科技有限公司 | Liquid crystal composition and light modulation device thereof |
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