CN110527436B - Special sealant for quantum dot packaging and preparation method thereof - Google Patents
Special sealant for quantum dot packaging and preparation method thereof Download PDFInfo
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- CN110527436B CN110527436B CN201910795792.9A CN201910795792A CN110527436B CN 110527436 B CN110527436 B CN 110527436B CN 201910795792 A CN201910795792 A CN 201910795792A CN 110527436 B CN110527436 B CN 110527436B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
Abstract
The invention discloses a special sealant for quantum dot packaging and a preparation method thereof, wherein the special sealant for quantum dot packaging comprises the following components in parts by mass: the component A comprises: 60-80 parts of organic silicon modified epoxy resin; 20-40 parts of a reactive diluent; 2-5 parts of a photoacid generator; 0.2-0.6 parts of a photosensitizer; the component B comprises: 60-80 parts of polyurethane modified organic silicon resin; 20-40 parts of an acrylate reactive diluent; 2-6 parts of a free radical photoinitiator; wherein the mass ratio of the component A to the component B is 4: 1-1: 2. The special sealant for quantum dot packaging has good compatibility with quantum dots, small influence on the fluorescence brightness of the quantum dots, excellent aging resistance, good bonding property and excellent environmental reliability.
Description
Technical Field
The invention relates to the field of quantum dot sealing materials, in particular to a special sealant for quantum dot packaging and a preparation method thereof.
Background
The appearance of the quantum dot technology enables the liquid crystal display technology to be upgraded and new breakthrough ports to be found, and the liquid crystal display technology is of great industrial interest. Since 2014, not only the international large factories such as samsung and LG are producing television display screens by quantum dot technology, but also the native manufacturers such as beijing oriental and huaxing photoelectricity in China declare that quantum dot backlight technology products are about to be introduced into mass production. At present, an important bottleneck still exists in the large-scale application of the quantum dot backlight source technology, namely the problem of the service life of the quantum dots which are main materials of the quantum dot backlight source technology. How to maintain long fluorescence lifetime in external environment is a key to whether the quantum dot backlight technology can be widely applied to economic and efficient display materials.
The encapsulating polymer utilizes the swelling-deswelling effect of the high molecular polymer to permeate and diffuse the quantum dots into the polymer, and the quantum dots are directly wrapped and contacted, so that the micro-scale encapsulation and isolation of the quantum dot nanoparticles are realized, the quantum dots are isolated from being contacted with the outside, the pollution of moisture, dust and the like is avoided, and the luminous performance and the service life of the quantum dot material are prolonged. Therefore, improving the water and oxygen barrier properties of the encapsulating polymer material and the composite strength between the quantum dot nanoparticles are crucial to prolonging the optical lifetime of the quantum dots
At present, the core technology of the quantum dot optical film sealing material is mainly mastered in few foreign companies (such as 3M, Dow and the like), and is blank at home, and downstream display screen manufacturing enterprises can only select foreign companies to cooperate. The future market prospect is very wide, the monopoly of foreign enterprises on the sealing material is broken, the localization of the quantum dot optical film is facilitated, and the technical level of the domestic new material industry is improved. For downstream industries, the method is beneficial to improving the competitiveness of the display screen manufacturing industry and promoting the domestic flat panel display industry to have profound significance for the domestic development of the flat panel display manufacturing industry in China. Therefore, a sealant special for quantum dot encapsulation suitable for quantum dot encapsulation is needed.
Disclosure of Invention
The invention aims to overcome at least one defect of the prior art and provides the special sealant for quantum dot packaging, which has good compatibility with quantum dots, small influence on the fluorescence brightness of the quantum dots, excellent aging resistance, good bonding property and excellent environmental reliability.
The invention also aims to provide a preparation method of the special sealant for quantum dot packaging.
The technical scheme adopted by the invention is as follows:
a special sealant for quantum dot packaging comprises the following components in parts by mass:
the component A comprises:
60-80 parts of organic silicon modified epoxy resin;
20-40 parts of a reactive diluent;
2-5 parts of a photoacid generator;
0.2-0.6 parts of a photosensitizer;
the component B comprises:
60-80 parts of polyurethane modified organic silicon resin;
20-40 parts of acrylate reactive diluent;
2-6 parts of a free radical photoinitiator;
wherein the mass ratio of the component A to the component B is 4: 1-1: 2.
The application takes two types of resins, namely a photocuring polyurethane modified organic silicon resin material and an organic silicon epoxy resin material which are independently synthesized by the Palema as main components, is matched with an active diluent and a photoinitiator, and is cured by hybrid light, so that the sealant realizes key performances of high water and oxygen isolation, light aging resistance, high transmittance, low fog degree, low volume shrinkage, strong cohesive force and the like, finally effectively solves the problem that the performance of quantum nanoparticles is reduced due to the permeation of water and oxygen, improves the fluorescence life of quantum dots, clears obstacles for the industrialization of quantum dot optical films, and further promotes the development of the local flat panel display industry.
Preferably, the mass ratio of the component A to the component B is 4: 1-2: 1. In the experimental process, the fact that when the mass ratio of the component A to the component B is 4: 1-2: 1, the resin and the quantum dots are excellent in compatibility (the sealant with poor compatibility is not beneficial to dispersion of the quantum dots, quenching of the quantum dots is easily caused, and the service life of the quantum dots is influenced) and can obtain a uniform stable solution, and the resin has small influence on the fluorescence brightness of the quantum dots and the fluorescence brightness of the quantum dots is high.
Preferably, the reactive diluent is 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexylformate or a mixture of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexylformate and poly [ (2-oxiranyl) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether. In the experimental process, the dispersion state of quantum dots in the organosilicon modified epoxy resin in different reactive diluents and the fluorescence brightness attenuation of a glue film are different, and the quantum dots are well dispersed in 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexyl formate or a mixture of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexyl formate and poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propylene glycol ether, so that a uniform and stable solution can be obtained, and the fluorescence brightness attenuation of the glue film is less.
Further preferably, the reactive diluent comprises 10-30 parts of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexyl formate and 0-20 parts of poly [ (2-oxiranyl) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether.
Preferably, the acrylate reactive diluent is one or more of isobornyl acrylate, tridecyl acrylate, dicyclopentadiene acrylate, tricyclodecane dimethanol diacrylate. The dispersion conditions and the fluorescence attenuation of quantum dots in the polyurethane modified organic silicon resin are different in different reactive diluents, and in the experimental process, the quantum dots are found to be in good dispersion states in isobornyl acrylate, tridecyl acrylate, dicyclopentadiene acrylate, tricyclodecane dimethanol diacrylate and the like, so that a uniform and stable solution can be obtained, and the fluorescence brightness attenuation of a glue film is also small. Further preferably, the acrylate reactive diluent is isobornyl acrylate and/or dicyclopentadiene acrylate.
Preferably, the photoacid generator is one or more of 4-isobutylphenyl-4 '-methylphenyliodiodohexafluorophosphate (IRGACURE 250), diphenyl- (4-phenylsulphur) phenylsulphonium hexafluorophosphate (GR-SS-002), bis (4,4' -thioethertriphenylsulphonium) hexafluoroantimonate and a mixture of diphenyl- (4-phenylsulphur) phenylsulphonium hexafluoroantimonate (UVI 6976). Wherein UVI 6976 is a mixture containing a portion of triarylsulfonium salt dimer, and is a solution dissolved in propylene carbonate, at a concentration of 50 wt.%
Preferably, the photosensitizer is one or more of 2-Isopropylthioxanthone (ITX), Camphorquinone (CM), Coumarin (CQ).
Preferably, the free radical photoinitiator is one or more of 2-hydroxy-2-methyl-1-phenyl-1-propanone (Darocur 1173), 1-hydroxycyclohexyl phenyl ketone (Irgacure 184), benzoin dimethyl ether (Irgacure 651), phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide (Irgacure 819).
The preparation method of the special sealant for quantum dot packaging comprises the following steps: and uniformly mixing the component A and the component B to obtain the special sealant for quantum dot packaging. The special sealant for quantum dot packaging does not need to use any auxiliary agent, and can be prepared by mixing the component A and the component B.
Compared with the prior art, the invention has the beneficial effects that: the invention uses special organosilicon modified epoxy resin and polyurethane modified organosilicon resin, so that the prepared sealant has high water and oxygen insulation performance and excellent light aging resistance, the free radical-cation hybrid ultraviolet curing technology is applied in the sealing material, the advantages of a free radical and cation light curing system are fully exerted, the respective defects are effectively avoided, and the sealing material has the advantages of high curing speed, large performance adjusting space, small curing shrinkage, strong adhesive force and the like.
Drawings
FIG. 1 is an infrared spectrum of an organosilicon modified epoxy resin.
FIG. 2 is an infrared spectrum of the polyurethane modified silicone resin.
Detailed Description
The examples of the present invention are provided for illustrative purposes only and are not to be construed as limiting the invention.
The starting materials used in the following examples were, unless otherwise specified, homogenized with a common commercially available product.
The silicone-modified epoxy resin described in the following examples is parylene EP550, which is prepared on a laboratory scale as follows:
(1) adding a certain amount of UVR-6100, tetra (dimethylsilyl) orthosilicate ester (the ratio of silicon hydrogen bond to unsaturated double bond is 1: 1.1) and 30ml of toluene into a 250ml four-mouth round-bottom flask (provided with a spherical condenser tube, a thermometer, a nitrogen tube and a dropping funnel), uniformly mixing, stirring, heating, adding the prepared chloroplatinic acid catalyst solution twice at the temperature of 30 ℃ and 50 ℃ (the chloroplatinic acid is dissolved by isopropanol in advance), reacting at 75 ℃, sampling at a certain time interval for FTIR test, and obtaining epoxy modified hydrogen-containing silicone oil when the characteristic absorption peak (1637-1640cm-1) of the double bond in a spectrogram disappears;
(2) adding a certain amount of mixed solution of epoxy modified hydrogen-containing silicone oil and toluene into a 250ml four-neck round-bottom flask (provided with a spherical condenser tube, a thermometer, a nitrogen tube and a dropping funnel), uniformly dropping the mixed solution of vinyl silicone oil (Mn 1000-2000) and toluene into the system by using the dropping funnel, adding a certain amount of catalyst chloroplatinic acid and polymerization inhibitor hydroquinone for reaction, reacting for 4-5H at 75-85 ℃, cooling to room temperature, and discharging to obtain the organosilicon modified epoxy resin, wherein the amount of the catalyst chloroplatinic acid is 0.3 percent of the mass of a reaction monomer, the polymerization inhibitor is 0.1 percent of the mass of the monomer, and the unsaturated double bond in the vinyl silicone oil and the n (Si-H): n (C): 1.0: 1.1 percent of the epoxy modified hydrogen-containing silicone oil are mixed.
The infrared spectrogram of the prepared organosilicon modified epoxy resin is shown in figure 1. As can be seen from FIG. 1, the double bond stretching vibration peak and the double bond C-H stretching vibration peak both disappeared, and Si-C, Si-O, the characteristic peak of epoxy and Si-OCH appeared3Characteristic peak of medium C-H, and 2920cm-1And (3) absorbing methylene stretching vibration absorption peaks, thereby proving that the organic silicon modified epoxy resin is successfully prepared.
The polyurethane modified silicone resin described in the following examples is lemma PU2386, which is prepared on a laboratory scale as follows:
sequentially adding the measured alpha, omega-dihydroxy polydimethylsiloxane, polyethylene glycol 400 and isophorone diisocyanate (n (NCO): n (OH): 4: 1) into a four-neck flask with a reflux condenser pipe, starting a stirrer for stirring, and heating in an oil bath; adding 0.05 percent (mass fraction) of catalyst DBTDL at 40 ℃, slowly heating to 60-65 ℃, then carrying out heat preservation reaction for 3-4 h, monitoring the content of isocyanate groups in the system by adopting a di-n-butylamine method, dropwise adding HEA (controlling the remaining N (NCO): n (OH): 1: 1.1-1.2) to carry out end-capping reaction when the content reaches 5-8 percent, dropwise adding at 40 ℃, carrying out dropwise adding for 0.5h, slowly heating to 75 +/-2 ℃ after dropwise adding, carrying out heat preservation reaction until the isocyanate groups react, and obtaining the double-bond end-capped organic silicon polyurethane resin.
The infrared spectrogram of the prepared polyurethane modified organic silicon resin is shown in figure 2. As can be seen from FIG. 2, 2270cm was not present in the spectrum-1The characteristic peak of-NCO at (A) indicates that no free-NCO group appears in the system; 809cm-1The infrared characteristic absorption peak of the C ═ C unsaturated double bond appears, which indicates that the photocurable C ═ C is successfully connected on the polymer molecular chain; 1542cm-1The absorption peak is a plane bending vibration peak of N-H; 1042cm-1The peak appeared here is the stretching vibration absorption peak of Si-O-Si; 3361cm-1The absorption peak is the stretching vibration peak of N-H on carbamate; 1730cm-1The absorption peak at (A) is attributed to the stretching vibration of C ═ O; 2957cm-1The vicinity is a stretching vibration peak of saturated C-H, which indicates that the polymer contains-CH3，-CH2-；1456cm-1Absorption indicates that the polymer contains benzene rings, and thus it is understood that the polymer has a desired structure.
Example 1
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging in the embodiment comprises the following steps: and uniformly mixing the component A and the component B according to the mass ratio of 3:1 to obtain the special sealant for quantum dot packaging.
Example 2
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
80 parts of organic silicon modified epoxy resin;
20 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 3
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
30 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 4
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
60 parts of organic silicon modified epoxy resin;
40 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 5
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
80 parts of organic silicon modified epoxy resin;
10 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
10 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propylene glycol ether;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 6
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
60 parts of organic silicon modified epoxy resin;
20 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
20 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 7
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
80 parts of polyurethane modified organic silicon resin;
20 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 8
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
UVI 69764 parts;
0.5 part of ITX;
(2) the component B comprises:
60 parts of polyurethane modified organic silicon resin;
40 parts of dicyclopentadiene acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 9
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of isobornyl acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 10
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
80 parts of polyurethane modified organic silicon resin;
20 parts of isobornyl acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 11
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
UVI 69764 parts;
ITX 0.5 part
(2) The component B comprises:
60 parts of polyurethane modified organic silicon resin;
40 parts of isobornyl acrylate;
darocur 11734 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 12
The composition and the preparation process of the sealant special for quantum dot packaging are basically the same as those of the sealant in the embodiment 1, and the difference is that the mass ratio of the component A to the component B in the embodiment 12 is 4: 1.
Example 13
The composition and the preparation process of the sealant special for quantum dot packaging are basically the same as those of the sealant in the embodiment 1, and the difference is that the mass ratio of the component A to the component B in the embodiment 13 is 1: 1.
Example 14
The composition and the preparation process of the sealant special for quantum dot packaging are basically the same as those of the sealant in the embodiment 1, and the difference is that the mass ratio of the component A to the component B in the embodiment 14 is 1: 2.
Example 15
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
GR-SS-0023 parts;
CQ 0.4 parts
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
irgacure 1842 parts;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Example 16
A special sealant for quantum dot packaging comprises the following components in parts by weight:
(1) the component A comprises:
70 parts of organic silicon modified epoxy resin;
15 parts of 3, 4-epoxy cyclohexyl methyl 3, 4-epoxy cyclohexyl formate;
15 parts of poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
2505 parts of IRGACURE;
CM 0.6 part
(2) The component B comprises:
70 parts of polyurethane modified organic silicon resin;
30 parts of dicyclopentadiene acrylate;
6515 parts of Irgacure;
wherein the mass ratio of the component A to the component B is 3: 1.
the preparation method of the sealant special for quantum dot packaging is the same as that of the embodiment 1, and the description is omitted here.
Comparative example 1
A sealant, the composition and preparation method of which are basically the same as those of the example, is different from that in the comparative example 1, polyurethane modified organic silicon resin CN990 of the company Saedoma is selected to replace the polyurethane modified organic silicon resin in the example 1.
Comparative example 2
A sealant having substantially the same composition and preparation method as those of the examples except that in comparative example 2, silicone-modified epoxy resin KR470, which is a silicone-modified silicone, was used instead of the silicone-modified epoxy resin in example 1.
Comparative example 3
A sealant, the composition and preparation method of which are substantially the same as those of the examples, except that in comparative example 3, the mass ratio of the component A to the component B is 1: 4.
In order to examine the performance of the sealant special for quantum dot encapsulation, the sealant special for quantum dot encapsulation prepared in examples 1 to 16 and the sealants of comparative examples 1 to 3 were subjected to performance tests, and the specific test method was as follows: will be provided withThe prepared glue is coated on the surface of the base material, the thickness of the coating is controlled to be about 10 mu m, and the glue layer is covered with another base material to prepare the attaching sheet. Irradiating and curing on a crawler-type photocuring machine of a 2X 1000W medium-pressure mercury lamp for 30S, wherein the maximum light intensity of the central position of an irradiation platform is 37.5mW/cm2. The hardness test was carried out in accordance with GB/T1730-93 "hardness test method for paint films". The cured packaging adhesive sheet is placed into an ultraviolet-visible spectrophotometer (TU-1810 type ultraviolet-visible spectrophotometer, Beijing Puproud analytical instruments Co., Ltd.) sample cell, and the light transmittance at the wavelength of 400nm is measured by using air as reference.
After the adhesive film is subjected to 1000h ultraviolet aging in a QUV/Spray ultraviolet accelerated aging test machine of Q-LAB company, a spectrophotometer is adopted to test delta b of white paper printed by brand-new A4.
The adhesive property test is as follows: and (3) placing the prepared attaching sheet in a high-temperature high-humidity box (85 ℃ and 85% RH) for 1000h, then placing the attaching sheet in boiling red ink for boiling for 3h, and observing whether the red ink permeates into the packaging layer by using a solid crystal microscope, thereby judging the bonding property of the sealant special for quantum dot packaging.
And (3) testing the water vapor transmittance: a sealant film having a thickness of 1mm was tested for Water Vapor Transmission Rate (WVTR) using a moisture vapor meter Mocon under the condition of 60 ℃/90% RH.
The results of the above performance tests are shown in table 1.
TABLE 1
As can be seen from the performance tests in Table 1, the special sealant for quantum dot packaging, prepared by the invention, has moderate hardness and good light transmittance, and also has good light transmittance after ultraviolet accelerated aging for 1000 hours, which indicates that the adhesive film has little yellowing and good weather resistance, and in addition, the adhesive property is also excellent, and particularly, when the mass ratio of the component A to the component B is 3:1, zero penetration of red ink can still be achieved after the component A is boiled in red ink for 3 hours. The prepared sealant special for quantum dot packaging has low water vapor transmission rate and excellent water and oxygen resisting performance.
The invention also tests the environmental reliability of the special sealant for quantum dot packaging, and relevant test methods and results are shown in table 2.
TABLE 2 detection of environmental reliability of sealants
The detection result of the environmental reliability of the sealant shows that the sealant can meet the actual production requirement.
The sealant disclosed by the invention can be produced in a large scale, a laboratory scale-up test is carried out from 500mL to 1000mL and from 2000mL to 100L, and the pilot scale is realized at present.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the technical solutions of the present invention, and are not intended to limit the specific embodiments of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention claims should be included in the protection scope of the present invention claims.
Claims (7)
1. The sealant special for quantum dot packaging is characterized by comprising the following components in parts by mass:
the component A comprises:
60-80 parts of organic silicon modified epoxy resin;
20-40 parts of a reactive diluent;
2-5 parts of a photoacid generator;
0.2-0.6 parts of a photosensitizer;
the component B comprises:
60-80 parts of polyurethane modified organic silicon resin;
20-40 parts of acrylate reactive diluent;
2-6 parts of a free radical photoinitiator;
wherein the mass ratio of the component A to the component B is 4: 1-1: 2;
the organic silicon modified epoxy resin is parylene EP550, and the polyurethane modified organic silicon resin is parylene PU 2386;
the active diluent is 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexyl formate or a mixture of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexyl formate and poly [ (2-oxiranyl) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether;
the acrylate reactive diluent is isobornyl acrylate and/or dicyclopentadiene acrylate.
2. The special sealant for quantum dot packaging according to claim 1, wherein the mass ratio of the component A to the component B is 4: 1-2: 1.
3. The sealant special for quantum dot encapsulation according to claim 1, wherein the reactive diluent comprises 10 to 30 parts of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexyl formate and 0 to 20 parts of poly [ (2-oxiranyl) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether.
4. The sealant special for quantum dot encapsulation according to claim 1, wherein the photoacid generator is one or more of 4-isobutylphenyl-4 '-methylphenyliodihexafluorophosphate, diphenyl- (4-phenylsulfanyl) phenylsulfonium hexafluorophosphate, a mixture of bis (4,4' -thioethertriphenylsulfonium) hexafluoroantimonate and diphenyl- (4-phenylsulfanyl) phenylsulfonium hexafluoroantimonate).
5. The sealant special for quantum dot encapsulation according to claim 1, wherein the photosensitizer is one or more of 2-isopropyl thioxanthone, camphorquinone and coumarin.
6. The sealant special for quantum dot encapsulation according to claim 1, wherein the radical photoinitiator is one or more of 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxycyclohexyl phenyl ketone, benzoin dimethyl ether and phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide.
7. The preparation method of the special sealant for quantum dot encapsulation as claimed in any one of claims 1 to 6, characterized by comprising the following steps: and uniformly mixing the component A and the component B to obtain the special sealant for quantum dot packaging.
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