CN102629027B - Orientation film, manufacture method thereof and liquid crystal display assembly - Google Patents

Orientation film, manufacture method thereof and liquid crystal display assembly Download PDF

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Publication number
CN102629027B
CN102629027B CN201110213616.3A CN201110213616A CN102629027B CN 102629027 B CN102629027 B CN 102629027B CN 201110213616 A CN201110213616 A CN 201110213616A CN 102629027 B CN102629027 B CN 102629027B
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temperature
precuring
liquid crystal
crystal display
alignment films
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CN201110213616.3A
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CN102629027A (en
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刘方兴
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BOE Technology Group Co Ltd
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Beijing BOE Optoelectronics Technology Co Ltd
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Abstract

The invention discloses an orientation film, a manufacture method thereof and a liquid crystal display assembly, which relate to the technical field of liquid crystal display and solve the problem that orientation films manufactured through the prior art are poor in thermology and mechanical performance. In a main curing step of the manufacture method of the orientation film, the existing single temperature heating method is replaced with a gradient temperature rising heating method, temperature difference between the a pre-curing step and the main curing step can be prevented from being overlarge, a curing effect of the orientation film is improved, and performance in the aspects such as thermology and mechanics of the orientation film after being cured are remarkably improved. Initial temperature of the gradient temperature is not high, temperature rises at a later stage, and power consumption when the temperature is low is smaller than that in the existing single high temperature curing process. If the manufacture method is utilized for a long time, a large amount of energy can be saved, and reducing of manufacture cost of a liquid crystal display device is achieved.

Description

Alignment films, its preparation method and LCD assembly
Technical field
The present invention relates to technical field of liquid crystal display, relate in particular to alignment films, its preparation method and LCD assembly.
Background technology
Polyimide (Polyimide, referred to as: PI) be one of best kind of thermotolerance in engineering plastics, because it also has good mechanical property, fatigue performance, dimensional stability and electrical property, the fields such as Aeronautics and Astronautics, microelectronics, nanometer, liquid crystal, diffusion barrier, laser are widely used in.
In field of liquid crystal display, alignment films is made up of PI material.Existing alignment films preparation method mainly comprises following 3 steps.
Coating composition step: the composition that comprises dicarboxylic anhydride compounds and diamine compounds is coated on liquid crystal display assembly.
Pre-cure step: above-mentioned composition is heated at the temperature of 70 DEG C to 80s (second).
Main curing schedule: to heating 1200s through pre-cure step above-mentioned composition after treatment at the temperature of 230 DEG C.
In the process of preparation alignment films, inventor finds: the alignment films that uses said method to prepare is performed poor in the performance of calorifics and terms of mechanics.
Summary of the invention
Embodiments of the invention provide a kind of alignment films and preparation method thereof, can improve thermal property and the mechanical property of alignment films.
For achieving the above object, embodiments of the invention adopt following technical scheme:
A preparation method for alignment films, comprising: application composition step, is coated in the composition that comprises dicarboxylic anhydride compounds and diamine compounds on liquid crystal display assembly; Pre-cure step is carried out heated at constant temperature at precuring temperature to described composition; Main curing schedule, taking described precuring temperature as basis, adopts the mode of gradient increased temperature to heat the described composition after precuring.
A kind of alignment films of being prepared by said method.
A kind of liquid crystal display assembly that is formed with above-mentioned alignment films.
In alignment films, its preparation method and LCD assembly that the embodiment of the present invention provides, in the preparation method's of alignment films main curing schedule, replace existing single temperature type of heating with the type of heating of gradient increased temperature, can prevent that the temperature contrast between pre-cure step and main curing schedule is excessive, therefore improved the solidification effect of alignment films, the performance of the aspect such as calorifics (thermotolerance), mechanics (toughness) of the alignment films after solidifying is significantly promoted.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the preparation method's of a kind of alignment films of the embodiment of the present invention process flow diagram;
Fig. 2 is the temperature-time curve figure of main curing schedule in the embodiment of the present invention.
Embodiment
The embodiment of the present invention provides a kind of preparation method of alignment films, comprising: application composition step, is coated in the composition that comprises dicarboxylic anhydride compounds and diamine compounds on liquid crystal display assembly; Pre-cure step is carried out heated at constant temperature at precuring temperature to described composition; Main curing schedule, taking described precuring temperature as basis, adopts the mode of gradient increased temperature to heat the described composition after precuring.
The embodiment of the present invention also provides a kind of alignment films of being prepared by said method.
The embodiment of the present invention provides again a kind of liquid crystal display assembly that is formed with above-mentioned alignment films.
In alignment films, its preparation method and LCD assembly that the embodiment of the present invention provides, in the preparation method's of alignment films main curing schedule, replace existing single temperature type of heating with the type of heating of gradient increased temperature, can prevent that the temperature contrast between pre-cure step and main curing schedule is excessive, therefore improved the solidification effect of alignment films, the performance of the aspect such as calorifics (thermotolerance), mechanics (toughness) of the alignment films after solidifying is significantly promoted.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
The embodiment of the present invention provides the preparation method of alignment films, and as shown in Figure 1, the method comprises the steps.
101, application composition step, is coated in the composition being made up of dicarboxylic anhydride compounds and diamine compounds on liquid crystal display assembly.
After dicarboxylic anhydride compounds mixes with diamine compounds, chemical reaction occurs, chemical equation is as follows:
In above formula, Section 1 is the molecular formula of dicarboxylic anhydride compounds from left to right, the molecular formula that Section 2 is diamine compounds from left to right, and the R in two molecular formula and R ' refer to two kinds of different aroma type chemical groups with phenyl ring; Arrow the right is the molecular formula of the polyamic acid of generation after dicarboxylic anhydride compounds reacts with diamine compounds.
102, pre-cure step is carried out heated at constant temperature at precuring temperature to described composition.
The object of precuring is remaining partial solvent after composition react to vapor away, and make coating the smooth densification of face, after precuring, also to check the effect of film coating, therefore this step can be same as the prior art: described composition is heated to 80s at the temperature of 70 DEG C, also can be: described composition is heated to 60~80s at the temperature of 70 DEG C.
Certainly, the value of precuring temperature is not limited to 70 DEG C that the embodiment of the present invention provides, and the duration of precuring process is also not limited to 60~80s that the embodiment of the present invention provides, precuring temperature and duration known to other any those skilled in the art may be used to the present invention.
103, main curing schedule, taking described precuring temperature as basis, adopts the mode of gradient increased temperature to heat the described composition after precuring.
Can there is cyclisation dehydration in the polyamic acid generating through reaction equation in step 101, form moisture and polyimide, can make moisture evaporation by the heating of this step, promotes the carrying out of cyclodehydration reaction.
The type of heating that this step adopts is different from the heated at constant temperature mode of existing main curing schedule, adopt the type of heating of gradient increased temperature, taking described precuring temperature as basis, main solidification process is divided into multiple time periods, temperature value in each time period is constant, temperature value in the next time period is higher than the temperature in the ongoing time period, until temperature reaches the PI film solidification temperature threshold value of appointment.
Existing main curing schedule is that 230 DEG C of PI film solidification temperature threshold values that directly temperature risen to appointment from precuring temperature 70 C after pre-cure step heat, temperature variation is violent, can cause between dicarboxylic anhydride compounds and diamine compounds react and cyclodehydration reaction accelerates suddenly or slack-off, easily make the thermotolerance (thermal property) of the polyimide generating reduce, also can reduce the pulling strengrth (mechanical property) of polyimide simultaneously.
By adopt the type of heating of gradient increased temperature in main curing schedule, can prevent that the temperature contrast between pre-cure step and main curing schedule is excessive, thereby avoid thermal property and the mechanical property variation of polyimide.
Wherein, at precuring temperature 70 C, the precuring time is while being 80s, the type of heating of gradient increased temperature (transverse axis represents the time of heating, and the longitudinal axis represents the temperature of heating, and s represents chronomere: second) as shown in Figure 2, specifically comprise: the described composition after precuring is heated 300 seconds successively at the temperature of 100 DEG C, at the temperature of 140 DEG C, heat 300 seconds, at the temperature of 180 DEG C, heat 300 seconds, at the temperature of 230 DEG C, heat 300 seconds.Experiment shows, adopts the PI film after these heating means are solidified, and aspect thermal property, glass temperature will exceed more than 20 DEG C than the glass temperature of the PI film after solidifying by prior art, and glass temperature is to weigh the leading indicator of PI heat resistance.Aspect mechanical property, the pulling strengrth of the PI film of manufacturing by prior art is in 100 about MPa to 180 MPas, and more than the pulling strengrth of PI film after above-mentioned heating means are solidified will promote 30 MPas, therefore mechanical property strengthens.
Main curing schedule is mainly in order to remove as early as possible moisture, to promote the carrying out of polyamic acid cyclodehydration reaction, is by its evaporation and remove good way of moisture.The initial temperature of main curing schedule is made as to 100 DEG C and has well solved the problem of removing moisture.100 DEG C time, moisture becomes gas evaporation, has both ensured removal moisture, has ensured that again initial temperature is unlikely to too high (less with the difference of precuring temperature).Certainly, initial temperature is preferably 100 DEG C, but is not limited to 100 DEG C, can be also that other can make moisture evaporation have the temperature that is unlikely to affect cyclodehydration reaction.
Experiment is found: when set temperature gradient, in the time that the temperature difference between guarantee gradient is consistent as far as possible, the solidification effect of composition is relatively good, four temperature as embodiment of the present invention setting: 100 DEG C, 140 DEG C, 180 DEG C and 230 DEG C, gradient is respectively: 140 DEG C-100 DEG C=40 DEG C, 180 DEG C-140 DEG C=40 DEG C and 230 DEG C-180 DEG C=50 DEG C, and 100 DEG C of initial temperatures are also only poor 30 DEG C apart from precuring temperature 70 C, between gradient, there is no obvious difference, thereby can ensure reacting and cyclodehydration course of reaction conditional relatively stable between dicarboxylic anhydride compounds and diamine compounds, be conducive to the carrying out of reaction.If gradient disparities is larger, may accelerate suddenly or slack-off because the flip-flop of reaction environment causes reaction, do not reach optimum response effect.
It should be noted that: in gradient increased temperature process, be not limited to only have above-mentioned four temperature, difference between each temperature is also not limited to describe difference above, the lasting time of each temperature is also not limited to the above-described time, also gradient increased temperature process that can be made up of other temperature, difference and duration, that can improve reaction effect.
In addition, because existing most of firing equipments all have the function that programmed control timing heats up, therefore the present invention only need can realize by formulation program the type of heating of gradient increased temperature, can not make because having increased thermograde solidification process become loaded down with trivial details.
In the preparation method's of the alignment films that the embodiment of the present invention provides main curing schedule, replace existing single temperature type of heating with the type of heating of gradient increased temperature, improve the solidification effect of PI, the performance of the aspect such as calorifics (thermotolerance), mechanics (toughness) of PI after solidifying is significantly promoted.And gradient increased temperature initial temperature is not high, the later stage is just raised to high temperature, and the more existing single hot setting process of power consumption when temperature is low is much smaller, as prolonged application can be energy-conservation in a large number, thereby realizes the reduction of the manufacturing cost of liquid crystal display.
The embodiment of the present invention also provides a kind of alignment films of being prepared by said method and is formed with the liquid crystal display assembly of this alignment films.
The embodiment of the present invention is mainly used in the manufacture of liquid crystal display.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, any be familiar with those skilled in the art the present invention disclose technical scope in; can expect easily changing or replacing, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should described be as the criterion with the protection domain of claim.

Claims (4)

1. a preparation method for alignment films, comprising: application composition step, is coated in the composition that comprises dicarboxylic anhydride compounds and diamine compounds on liquid crystal display assembly; Pre-cure step is carried out heated at constant temperature at precuring temperature to described composition, it is characterized in that, the preparation method of described alignment films also comprises main curing schedule:
Taking described precuring temperature as basis, adopt the mode of gradient increased temperature to heat the described composition after precuring;
Described taking described precuring temperature as basis, adopt the mode of gradient increased temperature to heat the described composition after precuring, comprise: the described composition after precuring is heated 300 seconds successively at the temperature of 100 DEG C, at the temperature of 140 DEG C, heat 300 seconds, at the temperature of 180 DEG C, heat 300 seconds, at the temperature of 230 DEG C, heat 300 seconds.
2. method according to claim 1, is characterized in that, described precuring temperature is 70 DEG C, and the precuring time is 60~80 seconds.
3. an alignment films, is characterized in that, is prepared by the method described in claim 1 or 2.
4. a liquid crystal display assembly, is characterized in that, is formed with alignment films claimed in claim 3.
CN201110213616.3A 2011-07-27 2011-07-27 Orientation film, manufacture method thereof and liquid crystal display assembly Expired - Fee Related CN102629027B (en)

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CN103033992A (en) * 2012-12-21 2013-04-10 京东方科技集团股份有限公司 Liquid crystal display substrate and preparation method thereof and liquid crystal display device
CN103359951B (en) * 2013-07-11 2015-10-14 北京京东方光电科技有限公司 A kind of film coating method, device and indicating meter
CN107622986B (en) * 2017-10-11 2019-08-30 扬州虹扬科技发展有限公司 A kind of high thermal conductivity, high voltage insulation rectifier bridge encapsulating structure and packaging method
CN114253034B (en) * 2021-12-20 2023-06-02 广州华星光电半导体显示技术有限公司 Liquid crystal alignment film, liquid crystal box, liquid crystal display device and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6350845B1 (en) * 1999-06-28 2002-02-26 Kaneka Corporation Polyimide compositions and novel acid dianhydrides to be used therein
CN1356585A (en) * 2000-11-24 2002-07-03 香港科技大学 Process for preparing optical orientation film
CN1862347A (en) * 2005-05-11 2006-11-15 京东方显示器科技公司 Method for forming alignment layer of LCD
CN101321845A (en) * 2005-12-01 2008-12-10 Lg化学株式会社 Method of producing liquid crystal aligning layer, liquid crystal aligning layer produced using the same, and liquid crystal display including liquid crystal aligning layer
CN101365769A (en) * 2006-01-04 2009-02-11 Lg化学株式会社 Composition for liquid crystal aligning, liquid crystal aligning layer manufactured by the same, and liquid crystal display comprising the same
CN101558100A (en) * 2007-01-09 2009-10-14 Lg化学株式会社 New copolyimide, liquid crystal aligning layer comprising the same, and liquid crystal display comprising the same

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6350845B1 (en) * 1999-06-28 2002-02-26 Kaneka Corporation Polyimide compositions and novel acid dianhydrides to be used therein
CN1356585A (en) * 2000-11-24 2002-07-03 香港科技大学 Process for preparing optical orientation film
CN1862347A (en) * 2005-05-11 2006-11-15 京东方显示器科技公司 Method for forming alignment layer of LCD
CN101321845A (en) * 2005-12-01 2008-12-10 Lg化学株式会社 Method of producing liquid crystal aligning layer, liquid crystal aligning layer produced using the same, and liquid crystal display including liquid crystal aligning layer
CN101365769A (en) * 2006-01-04 2009-02-11 Lg化学株式会社 Composition for liquid crystal aligning, liquid crystal aligning layer manufactured by the same, and liquid crystal display comprising the same
CN101558100A (en) * 2007-01-09 2009-10-14 Lg化学株式会社 New copolyimide, liquid crystal aligning layer comprising the same, and liquid crystal display comprising the same

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