CN1270979A - Organic silicon/epoxy resin packing material modified with nanometer-level silicon-base oxide - Google Patents
Organic silicon/epoxy resin packing material modified with nanometer-level silicon-base oxide Download PDFInfo
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- CN1270979A CN1270979A CN 00108814 CN00108814A CN1270979A CN 1270979 A CN1270979 A CN 1270979A CN 00108814 CN00108814 CN 00108814 CN 00108814 A CN00108814 A CN 00108814A CN 1270979 A CN1270979 A CN 1270979A
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Abstract
The present invention relates to a room temperature cured single-component organic silicon/epoxy resin encapsulating material after being activization-treated and modified with nanometer SiO2-x. The said encapsulating material contains modifier 0.3-4.5%, hexyl silicate as cross-linking agent 2.1-2.3%, low-molecular weight polyethylene wax and/or phthalate as plasticizer 1.4-1.7%, white carbon black as reinforcing agent 0-0.4% and assistant 0.1-0.3%. With the features of simple preparation process, room temperature curing, and short curing period, the encapsulating material may be used for encapsulating electronic and electric devices such as organic electroluminescent device (OELD), etc.
Description
The present invention relates to a kind of electric device package material, particularly relate to a kind of nanometer SiO that adopts process for treating surface that contains
2-xOrganosilicon/Resins, epoxy (PDMS/E of modification
44) single-component self-vulcanizing OELD device package material.
Organism electroluminescent device (OELD) is a kind of novel planar display device of present development newly developed, have open and driving voltage low, but and direct voltage drive, can be complementary with large-scale integrated circuit, easily realize full colorization, luminosity height (＞10
5Cd/m
2), quantum luminous efficiency height advantages such as (2.01m/w), but the OELD device can't satisfy application requiring work-ing life, wherein needing one of technical difficulty of solving is exactly the packaged material and the encapsulation technology of device.At present, abroad (Japan and the United States, Europe etc.) mainly adopt packaged materials such as Resins, epoxy, organosilicon and heat, light, radiation curing technology, but also there are many weak points, make Resins, epoxy embrittlement easy to crack, make degradation under the sealing property as the crazingization that produces owing to the internal stress effect.The packaged material of seeking to satisfy the OELD device performance becomes the focus and the key of current OELD device research and development.
Organosilicon superpolymer and Resins, epoxy all are the electric device package materials of often selecting for use in the electronic industry
[1.2]Organosilicon material has low temperature flexibility (Tg=-120 ℃), low surface energy, high temperature resistant, weather, corrosion-resistant, hydrophobic nature good, the dielectric strength advantages of higher, but also has the poor and wear resistance of mechanical mechanics property, anti-solvent, relatively poor, the more high shortcoming of cost of cohesive force.Resins, epoxy then has good mechanical property, chemical solvent resistance energy, antioxygen gas perviousness, water-repellancy, adhesiveproperties and better reaches easy machine-shaping, advantage such as with low cost, but since Resins, epoxy through with solidifying agent generation curing reaction after then form the 3 D stereo reticulated structure, lack relatively sliding between the macromolecular chain, and
C-CThe bond energy of the relative Si-O key with the C-O key of key is much smaller, and has higher surface energy, and has the polar hydroxyl on the macromolecular chain, thereby make it easily produce bigger internal stress, easy embrittlement behind the curing molding, the crazing degree is big, high temperature is degraded chain rupture easily down, is subject to water absorption and the reduction flexural strength
[3.4]
In recent years, extensively adopt modifying epoxy resin by organosilicon, promptly blend, copolymerization or the graft reaction by between the two reaches and can reduce the Resins, epoxy internal stress to form intramolecularly again toughness reinforcing, reaching reduction internal stress minimizing crazing reduces fragility, improve resistance to elevated temperatures, also improve organosilyl waterproof, grease proofing, antioxygen property simultaneously.Can form the 3 D stereo network structure with modifying epoxy resin by organosilicon, generate the Si-O key rigid structure of similar silicate sturcture, epoxide group scission of link introducing soft segment (Si-O-Si) reaches the intramolecularly toughening modifying simultaneously, can promote the consistency between the two-phase again, organosilicon is scattered among the Resins, epoxy better
[5.6]At present, use as electric device sealing material with modifying epoxy resin by organosilicon, generally the set time that needs long (several hrs was to several days), accelerate curing reaction, need be in the usage quantity of comparatively high temps (60 ℃ as for more than 100 ℃) or increase solidifying agent
[7], not only increase cost, but also be difficult to satisfy on the extensive device production line requirement (short, room temperature encapsulation of time) packaged material.Though also adopt photocuring packaging process and radiation curing packaging process
[8], but because required equipment costliness and processing requirement height, so fail extensively to adopt.Therefore, research and development can be at ambient temperature, and the electron device package material of quick-setting modifying epoxy resin by organosilicon has important Practical significance.The technological method of generally selecting for use all is to adopt the molecular structure that changes organosilane monomer or Resins, epoxy, thereby reduce stiff molecule group such as phenyl ring and introduce flexible group such as aliphatic chain and reach the reduction solidification value, accelerate the modification purpose of set time, but will cause the difficulty of synthon like this, make the monomer cost too high, also difficult large-scale production and application
[9]
Purpose of the present invention just provides a kind of new electric device package material, can make the packaging process of device simple, shorten set time, and at room temperature encapsulates and get final product.
The object of the present invention is achieved like this: utilize nano silicone base oxide (SiO
2-x) the quantum size characteristic of material, will be through the nanometer SiO after silane coupling agent carries out surface-active-treatment
2-xAdd organosilicon (PDMS) modified epoxy (E
44) in the packaging plastic matrix, because nanometer SiO
2-xSurfactivity is big, surface hydroxyl (OH) content height, can react coated one deck polar silanes long chain active group through surface grafting, can fully react with the free hydroxyl group in the matrix and form the three-dimensional network stiff molecule structure of masonry structure, thereby suppressing colloidal effectively flows, improve solidification rate, increase cohesive strength, shortened set time greatly; Simultaneously, because the nanometer quantum size effect has increased air-tightness
[10], the sealing property of packaging is significantly improved.Therefore, nano-material modified packaged material is to improve the packaged material performance and the practical method of modifying of a kind of easy, the easy row that reduces cost.
Main raw material(s) that the present invention relates to and reagent are selected as follows:
Hydroxyl-terminated injecting two methyl siloxane (PDMS), molecular weight are 4200, organic silicon chemical factory of Jilin Petroleum chemical industry group company; The positive own ester of silicic acid (C.P), Tianjin chemical reagent one factory; E
44Type Resins, epoxy (technical grade), Wuxi resin processing plant; Silane coupling agent, organic silicon chemical factory of Nanjing University; Dibutyl tin laurate (C.P), Tianjin chemical reagent factory; Nanometer SiO
2-x(20-50nm), Zhoushan, Zhejiang nano material tomorrow company; Ring ketone in the sixth of the twelve Earthly Branches (A.P); Dimethylbenzene (A.P); Chloroform (A.P); Dehydrated alcohol (A.P); Acetone (A.P).The raw-material producer that provides only is to illustrate supply channel, and not in restriction the present invention, and other producer chemical reagent with performance of the same name is all at the row of starting material involved in the present invention both at home and abroad.
Main technological route:
The preparation of packaged material is divided into two steps.The substrate material that at first prepares modifying epoxy resin by organosilicon adopts under the catalyst action, with hydroxyl and the Resins, epoxy (E in the organosilicon (PDMS)
44) in secondary hydroxyl or epoxy group(ing) open chemical bond generation dehydration reaction and form segmented copolymer.Then will be through the nanometer SiO of surfactivity polarity processing
2-xCompound is dispersed in the above-mentioned substrate material, heating make it with matrix in the free hydroxyl group generation dehydration reaction that exists, increase consistency, be uniformly dispersed and form stable three-dimensional net structure nanometer SiO
2-xModification (PDMS/E
44) composite encapsulating material.Nanometer SiO
2-x(the PDMS/E of modification
44) packaged material can be used for the room temperature fast-curing of OELD device, and check its sealing property.
The preparation of modifying epoxy resin by organosilicon substrate material:
With etc. the Resins, epoxy (E of weight ratio
44) ring ketone in the sixth of the twelve Earthly Branches solution and the xylene solution co-blended of organosilicon (PDMS) after add in three mouthfuls of neck flasks electromagnetic force heated and stirred, and drip the about 0.02-0.06 mole of catalyzer dibutyl tin laurate with separating funnel gradually.Heating reflux reaction, temperature of reaction remain on 120-150 ℃, and the reaction times is 8-10 hour.After reaction is finished, except that desolvating, then obtain the matrix (PDMS/E of modifying epoxy resin by organosilicon with underpressure distillation
44) colloid, its form is the light yellow transparent colloid of heavy-gravity.During actual production, can add a small amount of oxidation inhibitor (2,6-di-t-butyl-4-sylvan) and photostabilizer (benzophenone and benzotriazole category) by performance requriements.
Nanometer SiO
2-xSurfactivity polarity is handled:
In organo silane coupling agent solution, add and contain 3-5wt% nanometer SiO
2-xChloroformic solution, after fully disperseing with ultrasonic wave, reflux then, electromagnetic force stirs, controlled temperature is at 60-80 ℃, the time is 20-24 hour.Treat the intact postcooling of surface treatment to room temperature, filter then, separate, drying; With deionized water multipass filter wash repeatedly, regulating the pH value is 6-9, adopts the dehydrated alcohol processed at last, grinds to form fine powder after the drying and promptly gets surfactivity polar nanometer SiO again
2-xMaterial.
Adopt organosilicon alkanes coupling agent as nano based oxide compound (SiO
2-x) the surface-active-treatment agent, available general formula R SiX
3Expression.In the formula, X is the hydrolization group that is easy to that is combined on the Siliciumatom, as chloro (Cl), methoxyl group (OCH
3), oxyethyl group (OC
2H
5), methoxy ethoxy (OCH
3OC
2H
5), acetoxyl group (OCOCH
3) and the oxyethane methoxyl group, generate silanol-Si (OH) during hydrolysis
3And and SiO
2-xIn hydroxyl generation dehydration reaction and form the siloxanes of three-dimensional network shape.R is that vinyl or end (dividing α, β, γ position) have the carbochain of amino, epoxy group(ing), methacrylic acid group, sulfate etc., and its reactive group can react the back with the organic group in the resin and form chemical bond and combine.Nano silicon-based oxide (SiO
2-x) and the Resins, epoxy (E of organosilicon (PDMS) modification
44) can pass through silane coupling agent (RSiX
3) and combination, make when boundary lubrication takes place the improvement effect of mechanism performance to matrix material (inorganic-polymer), electrical specification remarkable.
Nanometer SiO
2-xQuantum size effect the temperature that set time of whole packaged material and curing process require is all had remarkable influence.General p-(the SiO that selects
2-x) type, its specific activity surface-area is 640 ± 5m
2/ g, The adsorbed hydroxyl content is 48, median size about 20nm, purity＞99.9, density＜0.15g/cm
3, narrow diameter distribution, and thing is non-crystalline state mutually.
Reactive force between the mutual accumulative hydrogen bond of nanoparticle surface is not strong, is easily separated to shear interaction force.Yet, these hydrogen bonds (nonbonding) can be externally shear action restore rapidly again after eliminating, make the reorganization of reuniting rapidly of its structure.This dependence time, the shearing force of reinstatement attitude reduction reaction was called " thixotropy " or " shear thinning behavior " with outer shear action." thixotropy " is nanometer SiO
2-xImprove the principal element of colloidal stroma material property.Because nanometer SiO
2-xHave three-dimensional network shape silica molecular structure, grand specific activity surface-area presents the serious coordinate bond deficiency in surface, and the extremely strong activity on surface appears in performance.But as nanometer SiO
2-xBefore being added in the matrix as additive, carrying out different surfactivity polarity at its surface physical property and handle, promoting the consistency between itself and the matrix, thereby reach uniformly dispersed, improve the thixotropic behavior purpose.General nanometer SiO after surface-active-treatment
2-xCan be divided into surperficial nonpolar nanometer SiO again
2-xWith surface polarity nanometer SiO
2-x, show following three specific characters:
1. surperficial lipophilicity: nanometer SiO
2-xAfter the processing of organo-silicon coupling agents such as silicone alkane, silazane, halosilanes,
Because one or more layers long-chain oleophylic alkyl of its outside surface " coverings ", so the nanometer SiO of formation
2-x
Have lipophilicity or hydrophobicity.
2. surface grafting reaction: when selected surface treatment agent molecule has two active group molecules, wherein
Group can with nanometer SiO
2-xThe surfactivity hydroxyl (OH) reaction, another group then can with
The polymer-based carbon qualitative response, thus play " bridge joint " effect, improve consistency between the two, increase
Dispersed.As the oxyethane methoxy silane, contain octene (ethene) base silane, thiirane methoxy
Base silane, oxabicyclo heptyl silane etc.
3. amphipathic: when selected surface treatment agent molecule has two above reactive groups, except it
In one can with nanometer SiO
2-xOutside the surface hydroxyl reaction, the existing wetting ability of rest activity group also has the parent
Oiliness, then gained nanometer SiO
2-xHas amphiphilic nature.
Adopt silane coupling agent as nanometer SiO in this experiment
2-xThe surface-active-treatment agent can form above-mentioned 1 type and 2 type effects.
Nanometer SiO after the surface-active-treatment
2-xAdd (PSMS/E
44) in the matrix colloid, nanometer SiO
2-xLast grafted alkyl lipophilic group can with (PDMS/E
44) alkyl (CH in the matrix
2,-CH
3), alkoxyl group (OCH
3) wait consistency well, impel SiO
2-xBe uniformly dispersed; While nanometer SiO
2-xLip-deep grafted epoxide group or unsaturated hydroxyl also can with (PSMS/E
44) hydroxyl generation dehydration reaction in the matrix on the macromolecular chain, make (PSMS/E
44) hydroxyl in the matrix disappears, and impels both compatible, dispersiveness also is greatly enhanced mutually.
Nanometer SiO
2-xModified organic silicon/Resins, epoxy prepares single-component self-vulcanizing packaging plastic:
Will be through the nanometer SiO after surfactivity polarity is handled
2-xAdd (PDMS/E by weight 0.3-4.5%
44) in the modified substrate, reflux, electromagnetic force stirs, 60-80 ℃ of temperature control, about time 12-48 hour, add linking agent (positive the own ester 2.1-2.3wt% of silicic acid), softening agent (the cured and/or phthalic ester 1.4-1.7wt% of low molecular polyethylene), strengthening agent (white carbon black 0-0.4wt%) and auxiliary agent (0.1-0.3wt%) simultaneously and be mixed with the self-vulcanizing packing colloid material of single-component, lucifuge sealing preservation.
Encapsulation step: adopting conventional self-vulcanizing encapsulation technology, specifically is under the room temperature vacuum state OELD device to be coated with envelope with glue spreading method.
Testing tool: Hitachi, FT-IR spectrograph, FT-Raman spectrograph
Nanometer (SiO
2-x) modification single-component self-vulcanizing (PDMS/E
44) composition of packing colloid material:
The key technical indexes of packaged material:
| The composition title | Volume content |
| (PDMS/E 44) matrix (1: 1-1.4) | ????92.0-96.0％ |
| Nanometer (SiO 2-x) (after the surface treatment) | ????0.3-4.5％ |
| Linking agent (the positive own ester of silicic acid) | ????2.1-2.3％ |
| Softening agent (the cured and/or phthalic ester of low molecular polyethylene) | ????1.4-1.7％ |
| Strengthening agent (white carbon black) | ????0-0.4％ |
| Other (auxiliary agent) | ????0.1-0.3％ |
| Mode of appearance | Light yellow transparent colloid |
| Density (g/cm 3) | 1.10-1.14 |
| Mobile (s) | 22-26 |
| Set time (h) | 2.0-2.5 |
| Shearing resistance (MPa) | 0.09-0.12 |
| Elasticity | Fine |
| Heat-resisting poach (90 ℃, 48 hours) | Do not find crackle (dried glue) |
| Tensile strength (Kg/cm 2) | 274-281 |
With not containing nanometer SiO
2-xThe PDMS/E of modification
44The packing colloid material directly encapsulates the green light OLED device of this prepared in laboratory, and cut-in voltage is V before the encapsulation
0=3.0-3.2V, I
0=0.371mA; The encapsulation back is the ability completely solidified after about 24 hours, and temperature needs 60-80 ℃ during curing, and the mensuration cut-in voltage is V
0'=9.3-9.6V, I
0'=4.456mA.Encapsulation is preceding at V
1=9.07V, I
1Under=the 2.42mA, surveying its high-high brightness is 3.1 * 70cd/m
2, after the encapsulation through 20 days at V
1'=9.08V, I
1It is 0.81 * 70cd/m that '=3.67mA surveys its high-high brightness again
2, illustrate without nanometer SiO
2-x(the PDMS/E of modification
44) encapsulation performance of packing colloid material is relatively poor, set time is longer.
With containing surface-active-treatment SiO
2-xPackaging plastic the green light OLED device of this prepared in laboratory is carried out package experiment check sealing property.The cut-in voltage of device is V before the encapsulation
0=3.0-3.2V, I
0=0.368mA; The cut-in voltage of encapsulated device is V
0'=4.1-4.2V, I
0'=0.373mA, packaged material required set time is 2.0-2.5 hour, solidifies to get final product under the room temperature vacuum condition.Device is at V before the encapsulation
i=9.02V, I
iTest brightness is 2.9 * 70Cd/m under the=1.38mA
2After 20 days, test (480h), V after the encapsulation
i=9.10V, I
i=2.49mA, brightness this moment is 2.5 * 70Cd/m
2Thereby the encapsulation material solidifies time can be shortened significantly, and the solidification value that requires when solidifying can be reduced to room temperature, OELD device sealing performance is significantly improved, increases the work-ing life of OELD device, the practicability of OELD device is had great importance.
From the above, of the present inventionly contain nanometer SiO after the surface treatment
2-xOrganosilicon/Resins, epoxy (PDMS/E of modification
44) single-component self-vulcanizing packaged material have preparation technology simple, reduce set time and solidify positive effects such as temperature required low, encapsulated device life-span length, excellent property.
Embodiment 1:
To be 1: 1 organosilicon (PDMS, molecular weight are 4200) and Resins, epoxy (E by weight ratio
44) each 6.5 gram, be dissolved in respectively in 10 milliliters of isopyknic dimethylbenzene and the cyclohexanone solvent, electromagnetic force stirs, temperature is 60 ℃, churning time is 4 hours, then above-mentioned solution is mixed to join in 100 milliliters the three neck round-bottomed flasks, electromagnetic force stirs, vary with temperature with separating funnel again and drip 0.01 mole of dibutyltin dilaurate catalyst gradually, final temp is controlled at 136 ℃, reacts 10 hours, treats to obtain shallow yellow transparent solution after back flow reaction is finished, remove solvent through underpressure distillation again, promptly obtain 10.3 gram modifying epoxy resin by organosilicon (PDMS/E
44) the matrigel material, its form is the light yellow transparent colloid material of heavy-gravity.
Embodiment 2:
2mlKH550 and 6mlKH560 mixed solvent (1: 3) add nanometer SiO in the 10ml chloroformic solution
2-x3 restrain, and after fully disperseing with ultrasonic wave, adopt reflux then, and electromagnetic force stirs, and temperature is controlled at 70 ℃, keeps 24 hours, and surface treatment is finished postcooling to room temperature, filtration, drying; With deionized water multipass filter wash repeatedly, regulating pH value is 7 again, adopts the dehydrated alcohol dehydration at last, grinds to form fine powder after the drying and promptly obtains 2.8 and restrain surfactivity polar nano silicon-based oxide SiO
2-x
Embodiment 3:
Will be through the nanometer SiO after surfactivity polarity agent KH560/KH550 (3: 1) handles
2-x2.7 gram adds 96 gram PDMS/E after joining in the 10ml chloroform solvent and fully dissolving dispersion with ultrasonic wave again
44In matrix (1: the 1) colloid; reflux then; electromagnetic force stirs, and is heated to 70 ℃ of controlled temperature, 48 hours reaction times; and under nitrogen protection, add the 2.1 own esters of positive silicic acid that restrain as linking agent; 1.5 gram low molecular polyethylene vinegar does not add white carbon black, adding assistant 10ml pimelinketone and dimethylbenzene (1: 1) mixed solvent; full and uniform stirring obtains the light yellow transparent colloid material of 98.4 grams after reacting completely.Through the test of OELD device package, OELD device cut-in voltage is V before the encapsulation
0=3.0-3.1V, I
0=0.417mA; Encapsulation back completely solidified after about 2.3 hours, measuring cut-in voltage again is V
0'=4.0-4.1V, I
0'=0.468mA.Encapsulation is preceding at V
1=10.02V, I
1Under=the 1.53mA, surveying its maximum height is 2.9 * 70cd/m
2, after the encapsulation through 20 days, at V
i=10.08V, I
iUnder=the 2.47mA, surveying its high-high brightness is 2.6 * 70cd/m
2, the functional of packing colloid material is described.
Embodiment 4:
Will be through the nanometer SiO after surfactivity polarity agent KH560/KH550 (3: 1) handles
2-x3.2 gram after fully dissolving disperses (ultrasonic wave) in the adding 10ml chloroform solvent, adds 95 gram (PDMS/E again
44) in matrix (1: the 1) colloid; reflux then; electromagnetic force stirs, and is heated to 60 ℃ of controlled temperature, 36 hours reaction times; and under nitrogen protection, add the 2.1 own esters of positive silicic acid that restrain as linking agent; 1.5 the gram low molecular polyethylene is cured, does not add white carbon black, adding assistant 10ml pimelinketone and dimethylbenzene (1: 1) mixed solvent; full and uniform stirring obtains the light yellow transparent colloid material of 97.2 grams after reacting completely.Through the test of OELD device package, OELD device cut-in voltage is V before the encapsulation
0=3.0-3.2V, I
0=0.342mA; Encapsulation back completely solidified after about 1.8 hours, measuring cut-in voltage again is V
0'=3.8-4.0V, I
0'=0.443mA.Encapsulation is preceding at V
1=10.01V, I
1Under=the 1.68mA, surveying its maximum height is 2.9 * 70cd/m
2, after the encapsulation through 20 days, at V
i=10.05V, I
iUnder=the 2.85mA, surveying its high-high brightness again is 2.7 * 70cd/m
2, the functional of packing colloid material is described.
Embodiment 5:
Will be through the nanometer SiO after surfactivity polarity agent KH560/KH550 (3: 1) handles
2-x4.6 after fully dissolving disperses (ultrasonic wave) in the gram adding 10ml chloroform solvent, add 97 gram (PDMS/E again
44) in matrix (1: the 1) colloid; reflux then, magnetic agitation is heated to 60 ℃ of controlled temperature; 14 hours reaction times; and under nitrogen protection, adding the 2.1 own esters of positive silicic acid that restrain as linking agent, 1.5 gram low molecular polyethylenes are cured, do not add white carbon black; adding assistant 10ml pimelinketone and dimethylbenzene (1: 1) mixed solvent; full and uniform stirring after reacting completely, obtains the light yellow transparent colloid material of 98.6 grams.Through the test of OELD device package, OELD device cut-in voltage is V before the encapsulation
0=3.0-3.2V, I
0=0.371mA; Completely solidified after encapsulating back 2.5 hours, measuring cut-in voltage again is V
0'=4.3-4.5V, I
0'=0.516mA.Encapsulation is preceding at V
1=10.01V, I
1Under=the 1.76mA, surveying its maximum height is 2.9 * 70cd/m
2, after the encapsulation through 20 days, at V
i=10.03V, I
iUnder=the 2.53mA, surveying its high-high brightness again is 2.6 * 70cd/m
2, the functional of packing colloid material is described.
Embodiment 6:
Will be through the nanometer SiO after the surfactivity polarity agent oxyethane methyl-monosilane coupling agent treatment
2-x2.3 after fully dissolving disperses (ultrasonic wave) in the gram adding 10ml chloroform solvent, add 94 gram (PDMS/E again
44) in matrix (1: the 1) colloid; reflux then, magnetic agitation is heated to 80 ℃ of controlled temperature; 24 hours reaction times; and under nitrogen protection, adding the 2.1 own esters of positive silicic acid that restrain as linking agent, 1.5 gram low molecular polyethylenes are cured, do not add white carbon black; adding assistant 10ml pimelinketone and dimethylbenzene (1: 1) mixed solvent; full and uniform stirring after reacting completely, obtains the light yellow transparent colloid material of 96.5 grams.Through the test of OELD device package, OELD device cut-in voltage is V before the encapsulation
0=3.0-3.2V, I
0=0.359mA; Completely solidified after encapsulating back 1.6 hours, measuring cut-in voltage again is V
0'=4.1-4.2V, I
0'=0.468mA.Encapsulation is preceding at V
1=10.01V, I
1Under=the 2.08mA, surveying its maximum height is 3.0 * 70cd/m
2, after the encapsulation through 20 days, at V
i=10.07V, I
iUnder=the 2.71mA, surveying its high-high brightness again is 2.8 * 70cd/m
2, the functional of packing colloid material is described.
Pertinent literature: [1] Wu Minyang, New Chemical Materials, 1998,27 (3): 22[2] synthetic resins, (day), 1998,44 (5): 19[3] Chu Jiurong, the polymer circular, 1999, (2): 66[4] Hou Qingpu, Huang Ying etc., polymer material science and engineering, 1997,13 (3): 45[5] Bavton B.L, J.Appl.Polgm.Sci.1993,47 (10): 18:1[6] Zhouning County's beautiful jade, Zhou Hong etc., thermosetting resin, 1996 (3): 25[7] Yao Kangde, Liu waits quietly, thermosetting resin, 1992, (3) 52[8] Li Shanjun, Yu Tao etc., thermosetting resin, 1997, (1) 8[9] Zhu Liusheng, Chen Huizong etc., the gluing jelly of China, 1993,2 (6): 8[10] Kasemura, T, Oshibe, etal, J.Adhension, 1990, (33): 19
Claims (4)
1, a kind of nanometer SiO that contains the processing of surfactivity polarity
2-xThe organosilicon of modification/epoxy-resin single-component self-vulcanizing packaged material, its weight consists of:
Organosilicon/epoxy matrix material of 92.0-96.0%,
The nanometer SiO of 0.3-4.5%
2Properties-correcting agent,
The own ester linking agent of the positive silicic acid of 2.1-2.3%,
Cured and/or the phthalate plasticizers of 1.4-1.7% low molecular polyethylene,
0-0.4% white carbon black strengthening agent,
The 0.1-0.3% auxiliary agent;
It is characterized in that: organosilicon in organosilicon/epoxy matrix material: the weight proportion of Resins, epoxy is
1: 1-1.4; Nanometer SiO
2-xBe the p type, its specific activity surface-area is 640 ± 5m
2/ g, The adsorbed hydroxyl content
Be 48, median size about 20nm, purity＞99.9, density＜0.15g/cm
3, narrow diameter distribution,
And thing is non-crystalline state mutually.
2, the nanometer SiO that contains the processing of surfactivity polarity as claimed in claim 1
2-xThe organosilicon of modification/epoxy-resin single-component self-vulcanizing packaged material is characterized in that: described nanometer SiO
2-xSurfactivity polarity treatment process as follows:
In silane coupling agent, add the p type nanometer SiO of 3-5wt%
2-xChloroformic solution, after fully disperseing with ultrasonic wave, reflux, electromagnetic force stirs, controlled temperature is at 60-80 ℃, the time is 12-24 hour; Treat the intact postcooling of surface treatment to room temperature, filtering separation then, drying; With deionized water multipass filter wash repeatedly, regulating pH value is 6-9 again, dewaters with dehydrated alcohol, grinds to form fine powder after the drying and promptly gets surfactivity polar nanometer SiO
2-xMaterial.
3, the nanometer SiO that contains the processing of surfactivity polarity as claimed in claim 2
2-xThe organosilicon of modification/epoxy-resin single-component self-vulcanizing packaged material is characterized in that: described silane coupling agent is available general formula R SiX
3Expression; X is the hydrolization group that is easy to that is combined on the Siliciumatom in the formula, as chloro (Cl), methoxyl group (OCH
3), oxyethyl group (OC
2H
5), methoxy ethoxy (OCH
3OC
2H
5), acetoxyl group (OCOCH
3) and the oxyethane methoxyl group etc., R is that vinyl or end (dividing α, β, γ position) have the carbochain of amino, epoxy group(ing), methacrylic acid group, sulfate etc.
4, a kind of as any one described nanometer SiO that contains the processing of surfactivity polarity of claim 1 to 3
2-xThe organosilicon of the modification/application of epoxy-resin single-component self-vulcanizing packaged material aspect the packaging electronic electric device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00108814 CN1118508C (en) | 2000-05-10 | 2000-05-10 | Organic silicon/epoxy resin packing material modified with nanometer-level silicon-base oxide |
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| CN 00108814 CN1118508C (en) | 2000-05-10 | 2000-05-10 | Organic silicon/epoxy resin packing material modified with nanometer-level silicon-base oxide |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1529807A3 (en) * | 2003-10-16 | 2006-01-25 | Nitto Denko Corporation | Epoxy resin composition for encapsulating optical semiconductor element and optical semiconductor device using the same |
| CN1302530C (en) * | 2003-06-11 | 2007-02-28 | 胜华科技股份有限公司 | Method for packaging electronic component |
| CN1311567C (en) * | 2001-01-02 | 2007-04-18 | 伊斯曼柯达公司 | Organic LED device with improved light efficiency |
| US7659012B2 (en) | 2004-02-02 | 2010-02-09 | Samsung Mobile Display Co., Ltd. | Organic electroluminescent display device |
| CN101525466B (en) * | 2009-04-03 | 2012-07-04 | 复旦大学 | Epoxy/organosilicon/inorganic nano-hybrid material, and preparation method and application thereof |
| CN102876282A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs |
| CN103208578A (en) * | 2013-03-21 | 2013-07-17 | 杭州杭科光电股份有限公司 | All-angle luminous light-emitting diode (LED) light source |
| CN103756615A (en) * | 2014-01-26 | 2014-04-30 | 江苏兴华胶带股份有限公司 | Polyolefin polymer modified binder material for organic electroluminescent device |
| CN103779508A (en) * | 2014-01-26 | 2014-05-07 | 江苏天楹之光光电科技有限公司 | Method for packaging electroluminescent diode |
| CN104152096A (en) * | 2014-01-26 | 2014-11-19 | 南通向阳光学元件有限公司 | Composite binder material used for packaging electroluminescent device and enclosing method thereof |
| CN104993067A (en) * | 2015-07-13 | 2015-10-21 | 深圳市华星光电技术有限公司 | Organic light-emitting diode package member and manufacture method thereof and display device |
| CN113930049A (en) * | 2021-10-20 | 2022-01-14 | 河南大学 | Spherical nano silicon dioxide epoxy resin slurry and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1311567C (en) * | 2001-01-02 | 2007-04-18 | 伊斯曼柯达公司 | Organic LED device with improved light efficiency |
| CN1302530C (en) * | 2003-06-11 | 2007-02-28 | 胜华科技股份有限公司 | Method for packaging electronic component |
| EP1529807A3 (en) * | 2003-10-16 | 2006-01-25 | Nitto Denko Corporation | Epoxy resin composition for encapsulating optical semiconductor element and optical semiconductor device using the same |
| US7659012B2 (en) | 2004-02-02 | 2010-02-09 | Samsung Mobile Display Co., Ltd. | Organic electroluminescent display device |
| CN1678140B (en) * | 2004-02-02 | 2010-11-03 | 三星移动显示器株式会社 | Organic electroluminescent display device |
| CN101525466B (en) * | 2009-04-03 | 2012-07-04 | 复旦大学 | Epoxy/organosilicon/inorganic nano-hybrid material, and preparation method and application thereof |
| CN102876282A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs |
| CN103208578A (en) * | 2013-03-21 | 2013-07-17 | 杭州杭科光电股份有限公司 | All-angle luminous light-emitting diode (LED) light source |
| CN103756615A (en) * | 2014-01-26 | 2014-04-30 | 江苏兴华胶带股份有限公司 | Polyolefin polymer modified binder material for organic electroluminescent device |
| CN103779508A (en) * | 2014-01-26 | 2014-05-07 | 江苏天楹之光光电科技有限公司 | Method for packaging electroluminescent diode |
| CN104152096A (en) * | 2014-01-26 | 2014-11-19 | 南通向阳光学元件有限公司 | Composite binder material used for packaging electroluminescent device and enclosing method thereof |
| CN103756615B (en) * | 2014-01-26 | 2015-02-04 | 江苏兴华胶带股份有限公司 | Polyolefin polymer modified binder material for organic electroluminescent device |
| CN104152096B (en) * | 2014-01-26 | 2015-09-23 | 南通向阳光学元件有限公司 | A kind of compoiste adhering agent material for electroluminescent device encapsulation and enclosure method |
| CN103779508B (en) * | 2014-01-26 | 2015-10-14 | 江苏天楹之光光电科技有限公司 | A kind of method for packing of electroluminescent diode |
| CN104993067A (en) * | 2015-07-13 | 2015-10-21 | 深圳市华星光电技术有限公司 | Organic light-emitting diode package member and manufacture method thereof and display device |
| CN113930049A (en) * | 2021-10-20 | 2022-01-14 | 河南大学 | Spherical nano silicon dioxide epoxy resin slurry and preparation method thereof |
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