CN104693467A - Method for controlling orientation of domains of liquid crystal polymer through anchoring effect of surface coating - Google Patents
Method for controlling orientation of domains of liquid crystal polymer through anchoring effect of surface coating Download PDFInfo
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- CN104693467A CN104693467A CN201510061036.5A CN201510061036A CN104693467A CN 104693467 A CN104693467 A CN 104693467A CN 201510061036 A CN201510061036 A CN 201510061036A CN 104693467 A CN104693467 A CN 104693467A
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Abstract
The invention discloses a method for controlling the orientation of the domains of a liquid crystal polymer through the anchoring effect of a surface coating. The method comprises the following steps: firstly, synthesizing liquid crystal monomers, polymerizing the liquid crystal monomers to obtain a liquid crystalline polymer, then dissolving the liquid crystalline polymer, coating the solution of the liquid crystalline polymer in a spinning way to obtain a liquid crystalline polymer film, coating the surface of the liquid crystalline polymer film in a spinning way, and annealing to obtain a liquid crystal polymer film with a strippable surface coating. The polarity of the surface coating does not need to be controlled, and the liquid crystal polymer with the surface coating is easy to obtain. Compared with a surface coating formed on a segmented copolymer film, the strippable surface coating can be removed easily without affecting the nature of the liquid crystal polymer so that the shape and appearance of the liquid crystal polymer can be researched conveniently. In addition, the liquid crystal monomer and the liquid crystal polymer can be synthesized easily, the method for controlling the anchoring orientation of the liquid crystal through the strippable surface coating can be used for preparing industrial nano materials, and because the surface coating is soluble and innoxious, the surface coating can be applied to biological materials and has potential application value.
Description
Technical field
The present invention relates to Material Field, particularly a kind of method being controlled the grappling effect adjustable liquid crystal display polymkeric substance farmland district orientation of liquid crystal unit by strippable top coat.
Background technology
Liquid crystal is a kind of extensive approved phenomenon in the orientation on the surface of mechanical friction, and be widely used in the manufacture of technique of display and equipment, therefore, the surface effects of liquid crystal and the Anchoring Effect of liquid crystal cause great interest in materials chemistry and physics.Liquid crystalline polymers combines the character of liquid crystal and polymkeric substance, and its body phase behavior and phase structure obtain to be studied widely, also obtains application in body by its mechanical property of tropism control.On the other hand, the arrangement in liquid crystal polymer film Zhong Chou district and orientation are subject to the impact of surface and interface, dissimilar surface, such as hard inorganic material, soft biological Link Port, can be used for the orientation behavior of inducing different types.Therefore, utilize interface effectiveness and surperficial effectiveness to regulate and control particular requirement that its farmland district orientation can meet thin-film device, has great importance.
Orientation and the stromal surface character of liquid crystal molecule have close relationship.Because liquid crystal in actual applications, all need regularly arranged, and its degree of orientation directly depend on the surface action of substrate.In order to realize the farmland district orientation of polymkeric substance in film, must suitable control film and interfacial interaction that is surperficial and substrate.In addition, other method is also used to the film obtaining long-range order recently, such as external magnetic field, shearing, solvent evaporation.Compared with those methods above-mentioned, the method for top coat is more effective, because it can be used for preparing industrialized nano material.The method of conventional surface coating is that the component of top coat has similar component to used block polymer, thus accurately can control the interface interaction between each component and coating of segmented copolymer, but, can only block polymer be applicable to, the farmland district orientation of homopolymer can not be controlled.Because Air Interface is to the Anchoring Effect of liquid crystal, the general vertical air interface of small molecules rod shaped liquid crystal primitive, and Air Interface is vertical with the normal orientation of liquid crystal laminate structure.When modifying free surface, the arrangement of small molecules rod shaped liquid crystal primitive will change.Therefore, at this, we attempt to utilize this principle, are controlled the orientation in liquid crystalline polymers farmland district by a kind of Anchoring Effect of top coat.This top coat can be removed very easily simultaneously, and convenient like this its pattern of directly research, is more conducive to obtaining pure single polymeric film.
Summary of the invention
The present invention is intended to the grappling orientation controlling liquid crystal by introducing the top coat easily peeled off, and provides a kind of Anchoring Effect by top coat to control the method for liquid crystalline polymers farmland district orientation.
Technical scheme of the present invention is:
Controlled a method for liquid crystalline polymers farmland district orientation by the Anchoring Effect of top coat, comprise the steps:
(1) liquid crystalline polymers is dissolved in chlorobenzene, polymers soln spin coating is obtained liquid crystal polymer film;
(2) after solvent volatilizees completely, then at liquid crystal polymer film surface spin coating top coat;
(3) then anneal, namely rear cooling of having annealed obtains the liquid crystal polymer film with peelable top coat.
Further, the structure of described liquid crystalline polymers is such as formula shown in I
Wherein R
1for the one in hydrogen, alkyl, R
2the one in hydrogen, alkyl or alkoxyl group, R
3it is the one in hydrogen, alkyl, alkoxyl group, nitro, cyano group, sulfonic group, halogen atom;
A is C or Si;
E is the one in a kind of in alkyl, alkoxyl group, ester group, carbonyl, amide group or their homologue or isomer;
for the one in formula II;
The preparation method of described liquid crystalline polymers is as follows:
The liquid crystal monomer of (a) synthesis containing double bond,
The structural formula of the described liquid crystal monomer containing double bond is such as formula shown in III
In formula III, wherein R
1for the one in hydrogen, alkyl,
R
2the one in hydrogen, alkyl or alkoxyl group,
R
3the one in hydrogen, alkyl, alkoxyl group, nitro, cyano group, sulfonic group, halogen atom,
E is the one in a kind of in alkyl, alkoxyl group, ester group, carbonyl, amide group or their homologue or isomer;
B above-mentioned monomer is polymerized by free radical polymerisation process and obtains liquid crystalline polymers by () under the condition of 50-150 DEG C.
Further, described strippable top coat is the one in Polyvinylpyrolidone (PVP), polymethylmethacrylate-methacrylic acid, sodium polymethacrylate and polyacrylamide, these peelable top coats have higher second-order transition temperature, better water-soluble, or some organic solvent can be dissolved in but immiscible with liquid crystalline polymers.
Further, the annealing temperature of described step (3) is 100-200 DEG C, and the time is 6-12min.
Further, the rate of temperature fall of described step (3) is 1-10 DEG C/min.
The present invention has following technique effect:
(1) the present invention introduces strippable top coat to control the grappling orientation of liquid crystalline polymers, and these coatings have excellent solvability and film-forming properties.
(2) the present invention is easy to the orientation controlling controlling farmland district, and determination methods is very simple, strippable top coat is utilized to control the grappling orientation of liquid crystalline polymers, by before and after annealing under ultraviolet/visible light the change of absorption peak and glancing incidence Wide angle X-ray diffraction test result judge the change of the arrangement of liquid crystalline polymers, and under ultraviolet/visible light, after comparing the peelable top coat of covering, locate change and the glancing incidence Wide angle X-ray diffraction test result of absorption peak, judge that this top coat controls the grappling change of liquid crystalline polymers.
(3) the present invention need not the polarity of control surface coating, and the composition of top coat is easy to obtain.Compared with the top coat be made up of segmented copolymer, the strippable top coat of the present invention is easily removed and is not affected the character of polymkeric substance, for the pattern studying liquid crystalline polymers is provided convenience.In addition, liquid crystal monomer of the present invention and polymkeric substance all easily synthesize, and connect the group with push-and-pull electronics at liquid crystal unit two ends, make it have larger polarizability, easy in like this electric field, and magnetic field polarization or self-assembling technique realize its orientation.In actual applications, regularly arranged liquid crystal molecule has larger using value.The grappling orientation being controlled liquid crystal by the method for peelable top coat can be used for preparing industrialized nano material, and because this top coat has solubility, the advantage of toxicological harmless, makes it on biomaterial, have potential using value.
Accompanying drawing explanation
Fig. 1 is the ultraviolet/visible absorbance figure before and after the liquid crystalline polymers annealing of uncoated soluble surface's coating in embodiment 1.
Fig. 2 is the ultraviolet/visible absorbance figure of the liquid crystalline polymers annealing front and back applying soluble surface's coating Polyvinylpyrolidone (PVP) in embodiment 1.
Fig. 3 is the glancing incidence Wide angle X-ray diffraction test result figure after the liquid crystalline polymers annealing of uncoated soluble surface's coating in embodiment 1.
Fig. 4 is the glancing incidence Wide angle X-ray diffraction test result figure after applying the annealing of soluble surface's coating Polyvinylpyrolidone (PVP) in embodiment 1.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further details, but the present invention is not limited to this.
Embodiment 1
A kind of liquid crystalline polymers, its structural formula is:
Raw material: to butylaniline, 1,10-dibromo-decane, potassium nitrite, hydrochloric acid, sodium hydroxide, methacrylic acid, DMF (DMF), tetrahydrofuran (THF) (THF), phenol, sherwood oil, chlorobenzene, Polyvinylpyrolidone (PVP).
Liquid crystal monomer; 10-[4-(4-phenoxy group) is to butyl nitrogen benzide] decyl-octyl methacrylate
First, by the method synthesis liquid crystalline polymers of liquid crystal monomer by radical polymerization, this liquid crystalline polymers is dissolved in chlorobenzene, liquid crystal polymer film is obtained through spin coating, its thickness at about 100-200nm, for the ease of comparative effectiveness, to a part of liquid crystal polymer film after evaporation of the solvent, at 130 DEG C, annealing was down to room temperature after 10 minutes, and then detecting liquid crystalline polymers farmland district is not having the arrangement before and after the annealing of overing number dissolubility top coat.Fig. 1 is the ultraviolet/visible absorbance figure before and after the liquid crystalline polymers annealing of uncoated soluble surface's coating in embodiment 1.As can be seen from Figure 1, the obvious absorption peak of azo primitive π-π * is had at 320nm place before the liquid crystalline polymers annealing of uncoated soluble surface's coating, after annealing, the intensity of azo primitive π-π * absorption peak significantly weakens, and can judge thus to be transformed into perpendicular to substrate by parallel substrate at the liquid crystal unit of liquid crystalline polymers in annealing process in liquid crystal polymer film of uncoated soluble surface's coating.Fig. 3 is the glancing incidence Wide angle X-ray diffraction test result figure after the liquid crystalline polymers annealing of uncoated soluble surface's coating in embodiment 1.As can be seen from Figure 3, structure in smectic after the liquid crystalline polymers annealing of uncoated soluble surface's coating, the normal direction of its smectic, perpendicular to substrate, supports the conclusion of " liquid crystalline polymers film in annealing process spontaneous formation liquid crystalline polymers farmland district nonplanar (vertically) orientation of uncoated soluble surface's coating " further.
Then to another part liquid crystalline polymers after evaporation of the solvent, do not anneal, directly be covered with soluble surface's coating Polyvinylpyrolidone (PVP) at film surface, then at 130 DEG C, annealing was down to room temperature after 10 minutes, then detected the arrangement of liquid crystalline polymers farmland district before and after the annealing of overing number dissolubility top coat.The normal direction that Fig. 4 shows its smectic is parallel to substrate.As can be seen from Figure 2, substantially do not change in the uv-absorbing intensity at 320nm place before and after the liquid crystalline polymers annealing of coating soluble surface coating Polyvinylpyrolidone (PVP), after this illustrates coating soluble surface coating Polyvinylpyrolidone (PVP), before and after annealing, liquid crystal unit is all be parallel to substrate.In addition, after removing top coat Polyvinylpyrolidone (PVP), this farmland district orientation arranged in parallel still can keep.
Embodiment 2
A kind of liquid crystalline polymers, its structural formula is:
Raw material: to butylaniline, 1,10-dibromo-decane, potassium nitrite, hydrochloric acid, sodium hydroxide, methacrylic acid, DMF (DMF), tetrahydrofuran (THF) (THF), phenol, sherwood oil, chlorobenzene, polyacrylamide.
Liquid crystal monomer; 10-[4-(4-phenoxy group) is to butyl nitrogen benzide] decyl-octyl methacrylate
First, by the method synthesis liquid crystalline polymers of liquid crystal monomer by radical polymerization, this liquid crystalline polymers is dissolved in chlorobenzene, liquid crystal polymer film is obtained through spin coating, its thickness at about 100-200nm, for the ease of comparative effectiveness, to a part of liquid crystal polymer film after evaporation of the solvent, at 130 DEG C, annealing was down to room temperature after 10 minutes, and then detecting liquid crystalline polymers farmland district is not having the arrangement before and after the annealing of overing number dissolubility top coat.Can find out in ultraviolet/visible absorbance figure.The obvious absorption peak of azo primitive π-π * is had at 320nm place before the liquid crystalline polymers annealing of uncoated soluble surface's coating, after annealing, the intensity of azo primitive π-π * absorption peak significantly weakens, and can judge that the liquid crystal unit in the liquid crystalline polymers annealing process of uncoated soluble surface's coating in liquid crystal polymer film is transformed into perpendicular to substrate by parallel substrate thus.Glancing incidence Wide angle X-ray diffraction test result is the structure of smectic after can finding out the liquid crystalline polymers annealing of uncoated soluble surface's coating, the normal direction of its smectic, perpendicular to substrate, supports the conclusion of " liquid crystalline polymers film in annealing process spontaneous formation liquid crystalline polymers farmland district nonplanar (vertically) orientation of uncoated soluble surface's coating " further.
Then to another part liquid crystalline polymers after evaporation of the solvent, do not anneal, directly be covered with soluble surface's coating polyacrylamide at film surface, then at 130 DEG C, annealing was down to room temperature after 10 minutes, then detected the arrangement of liquid crystalline polymers farmland district before and after the annealing of overing number dissolubility top coat.Can find out in ultraviolet/visible absorbance figure, substantially do not change in the uv-absorbing intensity at 320nm place before and after the liquid crystalline polymers annealing of coating soluble surface coating polyacrylamide, after this illustrates coating soluble surface coating polyacrylamide, before and after annealing, liquid crystal unit is all be parallel to substrate.In addition, after removing top coat polyacrylamide, this farmland district orientation arranged in parallel still can keep.
Embodiment 3
A kind of liquid crystalline polymers, its structural formula is:
Raw material: to butylaniline, 1,10-dibromo-decane, potassium nitrite, hydrochloric acid, sodium hydroxide, methacrylic acid, DMF (DMF), tetrahydrofuran (THF) (THF), phenol, sherwood oil, chlorobenzene, polymethylmethacrylate-methacrylic acid.
Liquid crystal monomer; 10-[4-(4-phenoxy group) is to butyl nitrogen benzide] decyl-octyl methacrylate
First, by the method synthesis liquid crystalline polymers of liquid crystal monomer by radical polymerization, this liquid crystalline polymers is dissolved in chlorobenzene, liquid crystal polymer film is obtained through spin coating, its thickness at about 100-200nm, for the ease of comparative effectiveness, to a part of liquid crystal polymer film after evaporation of the solvent, at 130 DEG C, annealing was down to room temperature after 10 minutes, and then detecting liquid crystalline polymers farmland district is not having the arrangement before and after the annealing of overing number dissolubility top coat.Can find out in ultraviolet/visible absorbance figure.The obvious absorption peak of azo primitive π-π * is had at 320nm place before the liquid crystalline polymers annealing of uncoated soluble surface's coating, after annealing, the intensity of azo primitive π-π * absorption peak significantly weakens, and can judge that the liquid crystal unit in the liquid crystalline polymers annealing process of uncoated soluble surface's coating in liquid crystal polymer film is transformed into perpendicular to substrate by parallel substrate thus.Glancing incidence Wide angle X-ray diffraction test result is the structure of smectic after can finding out the liquid crystalline polymers annealing of uncoated soluble surface's coating, the normal direction of its smectic, perpendicular to substrate, supports the conclusion of " liquid crystalline polymers film in annealing process spontaneous formation liquid crystalline polymers farmland district nonplanar (vertically) orientation of uncoated soluble surface's coating " further.
Then to another part liquid crystalline polymers after evaporation of the solvent, do not anneal, directly be covered with soluble surface's coating polymethylmethacrylate-methacrylic acid at film surface, then at 130 DEG C, annealing was down to room temperature after 10 minutes, then detected the arrangement of liquid crystalline polymers farmland district before and after the annealing of overing number dissolubility top coat.Can find out in ultraviolet/visible absorbance figure, substantially do not change in the uv-absorbing intensity at 320nm place before and after the liquid crystalline polymers annealing of coating soluble surface coating polymethylmethacrylate-methacrylic acid, after this illustrates coating soluble surface coating polymethylmethacrylate-methacrylic acid, before and after annealing, liquid crystal unit is all be parallel to substrate, in addition, remove top coat polymethylmethacrylate-methacrylic acid, this farmland district orientation arranged in parallel still can keep.
Embodiment 4
A kind of liquid crystalline polymers, its structural formula is:
Raw material: to butylaniline, 1,10-dibromo-decane, potassium nitrite, hydrochloric acid, sodium hydroxide, methacrylic acid, DMF (DMF), tetrahydrofuran (THF) (THF), phenol, sherwood oil, chlorobenzene, sodium polymethacrylate.
Liquid crystal monomer; 10-[4-(4-phenoxy group) is to butyl nitrogen benzide] decyl-octyl methacrylate
First, by the method synthesis liquid crystalline polymers of liquid crystal monomer by radical polymerization, this liquid crystalline polymers is dissolved in chlorobenzene, liquid crystal polymer film is obtained through spin coating, its thickness at about 100-200nm, for the ease of comparative effectiveness, to a part of liquid crystal polymer film after evaporation of the solvent, at 130 DEG C, annealing was down to room temperature after 10 minutes, and then detecting liquid crystalline polymers farmland district is not having the arrangement before and after the annealing of overing number dissolubility top coat.Can find out in ultraviolet/visible absorbance figure, the obvious absorption peak of azo primitive π-π * is had at 320nm place before the liquid crystalline polymers annealing of uncoated soluble surface's coating, after annealing, the intensity of azo primitive π-π * absorption peak significantly weakens, and can judge that the liquid crystal unit in the liquid crystalline polymers annealing process of uncoated soluble surface's coating in liquid crystal polymer film is transformed into perpendicular to substrate by parallel substrate thus.Glancing incidence Wide angle X-ray diffraction test result is the structure of smectic after can finding out the liquid crystalline polymers annealing of uncoated soluble surface's coating, the normal direction of its smectic, perpendicular to substrate, supports the conclusion of " liquid crystalline polymers film in annealing process spontaneous formation liquid crystalline polymers farmland district nonplanar (vertically) orientation of uncoated soluble surface's coating " further.
Then to another part liquid crystalline polymers after evaporation of the solvent, do not anneal, directly be covered with soluble surface's coating sodium polyacrylate at film surface, then at 130 DEG C, annealing was down to room temperature after 10 minutes, then detected the arrangement of liquid crystalline polymers farmland district before and after the annealing of overing number dissolubility top coat.Can find out in ultraviolet/visible absorbance figure.Substantially do not change in the uv-absorbing intensity at 320nm place before and after the liquid crystalline polymers annealing of coating soluble surface coating sodium polyacrylate, after this illustrates coating soluble surface coating sodium polyacrylate, before and after annealing, liquid crystal unit is all be parallel to substrate, in addition, after removing top coat sodium polyacrylate, this farmland district orientation arranged in parallel still can keep.
Claims (5)
1. controlled a method for liquid crystalline polymers farmland district orientation by the Anchoring Effect of top coat, it is characterized in that comprising the steps:
(1) liquid crystalline polymers is dissolved in chlorobenzene, polymers soln spin coating is obtained liquid crystal polymer film;
(2) after solvent volatilizees completely, then at liquid crystal polymer film surface spin coating top coat;
(3) then anneal, namely rear cooling of having annealed obtains the liquid crystal polymer film with peelable top coat.
2. the Anchoring Effect by top coat according to claim 1 controls the method for liquid crystalline polymers farmland district orientation, it is characterized in that: the structure of described liquid crystalline polymers is such as formula shown in I
Wherein R
1for the one in hydrogen, alkyl, R
2the one in hydrogen, alkyl or alkoxyl group, R
3it is the one in hydrogen, alkyl, alkoxyl group, nitro, cyano group, sulfonic group, halogen atom;
A is C or Si;
E is the one in a kind of in alkyl, alkoxyl group, ester group, carbonyl, amide group or their homologue or isomer;
for the one in formula II;
The preparation method of described liquid crystalline polymers is as follows:
The liquid crystal monomer of (a) synthesis containing double bond,
The structural formula of the described liquid crystal monomer containing double bond is such as formula shown in III
In formula III, wherein R
1for the one in hydrogen, alkyl,
R
2the one in hydrogen, alkyl or alkoxyl group,
R
3the one in hydrogen, alkyl, alkoxyl group, nitro, cyano group, sulfonic group, halogen atom,
E is the one in a kind of in alkyl, alkoxyl group, ester group, carbonyl, amide group or their homologue or isomer;
B above-mentioned monomer is polymerized by free radical polymerisation process and obtains liquid crystalline polymers by () under the condition of 50-150 DEG C.
3. the Anchoring Effect by top coat according to claim 1 and 2 controls the method for liquid crystalline polymers farmland district orientation, it is characterized in that: described strippable top coat is the one in Polyvinylpyrolidone (PVP), polymethylmethacrylate-methacrylic acid, sodium polyacrylate and polyacrylamide.
4. the Anchoring Effect by top coat according to claim 1 and 2 controls the method for liquid crystalline polymers farmland district orientation, it is characterized in that: the annealing temperature of described step (3) is 100-200 DEG C, and the time is 6-12min.
5. the Anchoring Effect by top coat according to claim 1 and 2 controls the method for liquid crystalline polymers farmland district orientation, it is characterized in that: the rate of temperature fall of described step (3) is 1-10 DEG C/min.
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| CN201510061036.5A CN104693467B (en) | 2015-02-05 | 2015-02-05 | The method that liquid crystal polymer farmland area orientation is controlled by the Anchoring Effect of face coat |
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| CN201510061036.5A CN104693467B (en) | 2015-02-05 | 2015-02-05 | The method that liquid crystal polymer farmland area orientation is controlled by the Anchoring Effect of face coat |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107121844A (en) * | 2017-05-23 | 2017-09-01 | 湘潭大学 | The method that the golden nanometer particle modified by liquid crystal polymer regulates and controls liquid crystal aligning |
| CN109575335A (en) * | 2018-11-12 | 2019-04-05 | 湘潭大学 | A method of regulation nanostructure orientation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020167639A1 (en) * | 2001-04-06 | 2002-11-14 | David Coates | Method of forming a liquid crystal polymer layer |
| CN101960367A (en) * | 2008-02-28 | 2011-01-26 | 夏普株式会社 | Composition for forming liquid crystal alignment film and liquid crystal display device |
-
2015
- 2015-02-05 CN CN201510061036.5A patent/CN104693467B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020167639A1 (en) * | 2001-04-06 | 2002-11-14 | David Coates | Method of forming a liquid crystal polymer layer |
| CN101960367A (en) * | 2008-02-28 | 2011-01-26 | 夏普株式会社 | Composition for forming liquid crystal alignment film and liquid crystal display device |
Non-Patent Citations (1)
| Title |
|---|
| TAKAHIRO SEKI: ""New strategies and implications for the photoalignment of liquid crystalline polymers"", 《POLYMER JOURNAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107121844A (en) * | 2017-05-23 | 2017-09-01 | 湘潭大学 | The method that the golden nanometer particle modified by liquid crystal polymer regulates and controls liquid crystal aligning |
| CN107121844B (en) * | 2017-05-23 | 2019-09-20 | 湘潭大学 | Regulate and control the method for liquid crystal aligning by the gold nanoparticle that liquid crystal polymer is modified |
| CN109575335A (en) * | 2018-11-12 | 2019-04-05 | 湘潭大学 | A method of regulation nanostructure orientation |
| CN109575335B (en) * | 2018-11-12 | 2021-07-30 | 湘潭大学 | Method for regulating and controlling orientation of nano structure |
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