Frame-sealing adhesive composition, method of preparing the same, and display apparatus
09574133 ยท 2017-02-21
Assignee
- Boe Technology Group Co., Ltd. (Beijing, CN)
- Beijing Boe Optoelectronics Technology Co., Ltd. (Beijing, CN)
Inventors
Cpc classification
C09K2211/1044
CHEMISTRY; METALLURGY
C09K2211/1029
CHEMISTRY; METALLURGY
C09J4/00
CHEMISTRY; METALLURGY
B32B2307/422
PERFORMING OPERATIONS; TRANSPORTING
B32B2457/202
PERFORMING OPERATIONS; TRANSPORTING
C09J9/00
CHEMISTRY; METALLURGY
B32B2307/714
PERFORMING OPERATIONS; TRANSPORTING
C08K5/45
CHEMISTRY; METALLURGY
B32B7/12
PERFORMING OPERATIONS; TRANSPORTING
C09K2211/1092
CHEMISTRY; METALLURGY
International classification
C09J9/00
CHEMISTRY; METALLURGY
B32B7/12
PERFORMING OPERATIONS; TRANSPORTING
Abstract
A frame-sealing adhesive composition and a method of preparing the same. The frame-sealing adhesive composition includes 1.45 wt % to 1.65 wt % of photochromic molecules based on the total weight of the frame-sealing adhesive composition, said photochromic molecules are inert to polymeric materials. The method of producing a frame-sealing adhesive composition includes mixing 1.45 wt % to 1.65 wt % of photochromic molecules based on the total weight of the frame-sealing adhesive composition with a frame-sealing adhesive to form a stirred mixture; and degassing the stirred mixture.
Claims
1. A frame-sealing adhesive composition comprising: 1.45 wt % to 1.65 wt % of photochromic molecules based on the total weight of the frame-sealing adhesive composition, wherein the photochromic molecules are inert to polymeric materials; wherein the photochromic molecules are represented by the structural formula of: ##STR00007## wherein R.sup.1 is ethyl; R.sup.2 is hydrogen, hydroxyphenyl, methyl, ethyl or methoxy; R.sup.3 is methyl or ethyl; and X is N.
2. The frame-sealing adhesive composition of claim 1, wherein the photochromic molecules comprises 1.55 wt % to 1.60 wt % based on the total weight of the frame-sealing adhesive composition.
3. The frame-sealing adhesive composition of claim 1, wherein the photochromic molecules are diarylethylene-based compounds.
4. A display apparatus, comprising two substrates assembled together, wherein the two substrates assembled together are bonded with the frame-sealing adhesive composition of claim 1.
5. A method of preparing a frame-sealing adhesive composition comprising: adding 1.45 wt % to 1.65 wt % of photochromic molecules based on the total weight of the frame-sealing adhesive composition into a frame-sealing adhesive and stirring the mixture to form a stirred mixture, wherein the photochromic molecules are inert to polymeric materials; and degassing the stirred mixtures; wherein the photochromic molecules are represented by the structural formula of: ##STR00008## wherein R.sup.1 is ethyl; R.sup.2 is hydrogen, hydroxyphenyl, methyl, ethyl or methoxy; R.sup.3 is methyl or ethyl; and X is N.
Description
DETAILED DESCRIPTION OF THE INVENTION
(1) To address the prior art problem that observation precision of sealant is relatively low, thereby resulting in the technical problems of product defects, the embodiments of the present invention provide a sealant composition, a method of preparing the same, and a display apparatus. In the sealant composition of the embodiment of the present invention, 1.45 wt % to 1.65 wt % of photochromic molecules are added based on the total weight of the sealant composition. Thus, when testing the defects of sealant, the photochromic molecules emit fluorescence under UV radiation so as to improve the precision of observing the sealant, facilitating clearly finding impurities, punctures, holes, and edge morphometry in the sealant, and improving the analysis precision. For describing the object, technical solution, and advantages of the present invention more detailedly, the following examples are provided to further illustrate the present invention.
(2) An embodiment of the present invention provides a frame-sealing adhesive composition comprising: 1.45 wt % to 1.65 wt % of photochromic molecules which are inter when compounding polymeric materials, based on the total weight of the frame-sealing adhesive composition.
(3) In the embodiments of the present invention, the components of the frame-sealing adhesive composition are the same as those of the prior art frame-sealing adhesive, except incorporating 1.45 wt % to 1.65 wt % of photochromic molecules which are inert in the compounding of polymeric materials. In other words, when the frame-sealing adhesive composition undergoes photocuring and thermal curing, the photochromic molecules will not react with any other component of the frame-sealing adhesive composition, but be directly dispersed in a form of molecules within the frame-sealing adhesive composition. In the embodiments of the present invention, the frame-sealing adhesive composition comprises the photochromic molecules present therein. Therefore, when the frame-sealing adhesive is observed with microscope, a beam of LTV radiation is introduced on the observation zone of microscope. The photochromic molecules emit fluorescence under UV radiation, thereby facilitating finding out the defects of frame-sealing adhesive composition, such as impurities, punctures, holes, etc.; facilitating observing the edge morphometry, and improving the analysis precision of frame-sealing adhesive. Moreover, the photochromic molecules in the holes exhibit various fluorescent brightness due to the barrier of holes, and thus the imaging of frame-sealing adhesive exhibit better three-dimensional effect, thereby facilitating the observation of morphometry of frame-sealing adhesive and improving the observation precision of frame-sealing adhesive. Furthermore, using such frame-sealing adhesive composition allows to avoid adjusting microscope lens and filters upon observation by using conventional microscopes, saving the process time, improving the analysis efficiency of frame-sealing adhesive defects, thereby improving the yield of products.
(4) Preferably, the photochromic molecules comprise 1.55 wt % to 1.60 wt % based on the total weight of the frame-sealing adhesive composition.
(5) In the embodiments of the present invention, adding an excess of photochromic molecules may result in a decrease of bonding property of the frame-sealing adhesive composition; and adding an insufficient amount of photochromic molecules may result in too diluent distribution of photochromic molecules in the frame-sealing adhesive composition, thereby making against the observation of morphometry of frame-sealing adhesive. Thus, it is necessary to add an appropriate amount of photochromic molecules. The inventors find through experiments that the photochromic molecules can comprise 1.45 wt % to 1.65 wt % based on the total weight of the frame-sealing adhesive composition, preferably 1.55 wt % to 1.60 wt % of based on the total weight of the frame-sealing adhesive composition, e.g., 1.45 wt %, 1.48 wt %, 1.50 wt %, 1.55 wt %, 1.58 wt %, 1.60 wt %, 1.62 wt % or 1.65 wt % based on the total weight of the frame-sealing adhesive composition.
(6) Preferably, the photochromic molecules are diarylethylene-based compounds.
(7) In the embodiments of the present invention, diarylethylene-based compounds can be used as the photochromic molecules. Since the diarylethylene-based compounds have good thermal stability, quick response, and relatively high quantum yield. Thus, when the frame-sealing adhesive composition undergoes thermal curing, it can maintain the stability of molecules; when the frame-sealing adhesive undergoes defect analysis, it exhibits quick response, and high fluoroscence brightness, thereby facilitating the observation of frame-sealing adhesive. Other photochromic molecules, such as fulgide, can also be used in the frame-sealing adhesive composition of the embodiments of the present invention.
(8) Preferably, the diarylethylene-based compounds are represented by the structural formula of:
(9) ##STR00003##
wherein R.sup.1 is methyl or ethyl; R.sup.2 is hydrogen, hydroxyphenyl, methyl, ethyl, methoxy or halogen atom; R.sup.3 is hydrogen, methyl or ethyl; and X is N or S.
(10) As shown in the following structural formula, the left is the open-ring state of the diarylethylene-based compounds, which is colorless; and the right is the closed-ring state of the diarylethylene-based compounds upon being radiated with UV light having a specific wavelength, which is purple. Through the purple fluoroscence emitted by the compound, the frame-sealing adhesive is observed for morphometry with higher precision of observation and higher precision of analysis.
(11) ##STR00004##
wherein R.sub.1, R.sub.2, R.sub.3 and X are defined as above.
(12) Preferably, the diarylethylene-based compounds are particularly represented by the structural formula of:
(13) ##STR00005##
wherein R.sup.1 is methyl; R.sup.2 is Cl; R.sup.3 is H; and X is S.
(14) The embodiments of the present invention further provide a display apparatus comprising two substrates assembled together, wherein the two substrates assembled together are bonded with any of the frame-sealing adhesive compositions of the aforesaid embodiments of the present invention. The display apparatus can be any product or part having a display function, such as liquid crystal panel, electronic paper, OLED panel, mobile, tablet PC, television, display, notebook, digital frame, navigator, and the like.
(15) The embodiments of the present invention further provide a method of preparing the frame-sealing adhesive composition comprising:
(16) adding 1.45 wt % to 1.65 wt % of photochromic molecules into a frame-sealing adhesive based on the total weight of the frame-sealing adhesive composition and stirring the mixture to form a stirred mixture, wherein the photochromic molecules are inert in compounding polymeric materials; and
degassing the stirred mixture.
(17) In the method of preparing the frame-sealing adhesive composition of the embodiments of the present invention, the photochromic molecules which is inert in the compounding of polymer are first mixed with other components of the frame-sealing adhesive by stirring, and then degassed to form the frame-sealing adhesive composition. Since the photochromic molecules are incorporated into the frame-sealing adhesive composition, the observation zone of microscope is subject to UV radiation when the cured frame-sealing adhesive composition is observed under microscope. The photochromic molecules fluorosce under UV radiation, thereby facilitating the observation of morphometry of selant, facilitating screening out the defectivly bonding product of frame-sealing adhesive, improving the pass ratio of product, avoiding the need of adjusting the lens of microscope and the filters, and simplifying the operation of analysis.
(18) The defects of the frame-sealing adhesive composition of the embodiments of the present invention can be examined under the following devices: said devices comprise a microscope, as well a UV lamp from which UV light is emitted for radiating the observation zone of microscope.
(19) Preferably, the light emitted from the UV lamp forms an angle of from 45 to 90 with regard to the plane of the observation zone of the microscope.
(20) The following examples are provided to further illustrate the frame-sealing adhesive composition and the method of preparing the same of the embodiments of the present invention. However, the present invention is not limited to the following examples. The following examples utilize only preferable materials as the components of the frame-sealing adhesive, wherein the frame-sealing adhesive is available from Mitsui Chemical Inc. under the trademark of NO2920; and the added photochromic molecules are diarylethylene-based compounds. The substituents of R.sup.1, R.sup.2, and R.sup.3 in the specific photochromic molecules and the weight percent of the photochromic molecules are listed in Table below.
(21) To the frame-sealing adhesive as list in Table 1, various weight percents of diarylethylene-based compounds are added and stirred at a temperature of, preferably, from 10 C. to 30 C. for 30 to 60 min (e.g., stirred at 29 C. for 30 min, at 18 C. for 45 min, or at 20 C. for 60 min, preferably, stirred at 20 C. for 60 min) to form a stirred mixture. The diarylethylene-based compounds are represented by the structural formula of:
(22) ##STR00006##
wherein the selected substituents of R.sup.1, R.sup.2, R.sup.3, X and F.sub.2 are listed in Table 1.
(23) The stirred mixture as described above can be degassed by using, e.g., the degassing machine under the model SIENOX.
(24) Examination and Analysis Test of Defects
(25) Each frame-sealing adhesive composition as described was applied onto a substrate, and subject to cell assembly with another substrate under vacuum. Then, the assembled cell underwent photocuring under UV radiation for 30 min, followed by thermal curing for 60 min. A microscope was used to examine the defects of frame-sealing adhesive. Upon observation, the observation zone of the microscope was radiated with UV light having a wavelength as listed in Table 1.
(26) TABLE-US-00001 TABLE 1 Components and Effect Evaluation of Frame-sealing adhesive Composition Weight UV Percent of Wavelength Frame-sealing Photochromic Photochromic Upon Results of Ex. adhesive Molecules Molecules Observation Observation 1 to 5 NO2920 R.sup.1 is methyl; R.sup.2 is 1.25 wt % 365 nm Unclear difference methyl; R.sup.3 is hydrogen; of morphometry and X is S 1.45 wt % Visible difference of morphometry 1.50 wt % Visible difference of morphometry 1.65 wt % Clear difference of morphometry 3.00 wt % Unclear difference of morphometry 6 to 11 NO2920 R.sup.1 is ethyl; R.sup.2 1.45 wt % 365 nm Visible difference hydroxyphenyl; R.sup.3 is of morphometry methyl; and X is N 1.55 wt % Clear difference of morphometry 1.60 wt % Clear difference of morphometry 1.65 wt % Visible difference of morphometry 1.75 wt % Unclear difference of morphometry 2.50 wt % Unclear difference of morphometry 12 to 16 NO2920 R.sup.1 is methyl; R.sup.2 is 0.05 wt % 365 nm Unclear difference chloro; R.sup.3 is hydrogen; of morphometry and X is S 1.35 wt % Unclear difference of morphometry 1.45 wt % Visible difference of morphometry 1.52 wt % Clear difference of morphometry 1.65 wt % Visible difference of morphometry 17 to 22 NO2920 R.sup.1 is ethyl; R.sup.2 is 0.50 wt % 365 nm Unclear difference methoxy; R.sup.3 is of morphometry hydrogen; and X is N 1.45 wt % Visible difference of morphometry 1.48 wt % Visible difference of morphometry 1.58 wt % Clear difference of morphometry 1.65 wt % Clear difference of morphometry 1.85 wt % Unclear difference of morphometry 23 to 27 NO2920 R.sup.1 is methyl; R.sup.2 is 1.45 wt % 365 nm Unclear difference ethyl; R.sup.3 is ethyl; and X of morphometry is S 1.55 wt % Clear difference of morphometry 1.58 wt % Clear difference of morphometry 1.60 wt % Clear difference of morphometry 1.75 wt % Unclear difference of morphometry
(27) It can be seen from the aforesaid Examples 1 to 27 that the incorporation of photochromic molecules into the frame-sealing adhesive composition facilitates observing the morphometry of frame-sealing adhesive, especially facilitates finding out defects, such as punctures and holes, of the frame-sealing adhesive so as to pick out defective products in good time and improve the pass ratio of product. Moreover, the added photochromic molecules does not affect the bonding property of the original frame-sealing adhesive.
(28) The incorporation of photochromic molecules into the frame-sealing adhesive composition of the embodiments of the present invention facilitates observing the frame-sealing adhesive with better precision, and allows to avoid the need of adjusting the lens of microscope and the filters, thereby simplifying the operation of analysis.
(29) It is apparent that persons skilled in the art can make various modifications and variations to the present invention without departing from the spirit and scope of the present invention. Thus, provided that such modifications and variations of the present invention fall within the scope of the appended claims and their equivalences, the present invention also encompasses these modifications and variations.