CN106832955A - A kind of LED encapsulation organic siliconresin and preparation method thereof - Google Patents
A kind of LED encapsulation organic siliconresin and preparation method thereof Download PDFInfo
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- 238000005538 encapsulation Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 150000001336 alkenes Chemical class 0.000 claims abstract description 78
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 78
- 239000010432 diamond Substances 0.000 claims abstract description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- YLJJAVFOBDSYAN-UHFFFAOYSA-N dichloro-ethenyl-methylsilane Chemical compound C[Si](Cl)(Cl)C=C YLJJAVFOBDSYAN-UHFFFAOYSA-N 0.000 claims abstract description 11
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 239000005055 methyl trichlorosilane Substances 0.000 claims abstract description 11
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005054 phenyltrichlorosilane Substances 0.000 claims abstract description 10
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000004132 cross linking Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 54
- 238000004140 cleaning Methods 0.000 claims description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 35
- 238000005406 washing Methods 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 30
- 239000003513 alkali Substances 0.000 claims description 25
- 239000003960 organic solvent Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 11
- 239000005046 Chlorosilane Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 10
- 235000021110 pickles Nutrition 0.000 claims description 10
- 238000005554 pickling Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000005292 vacuum distillation Methods 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 238000007711 solidification Methods 0.000 claims description 8
- 230000008023 solidification Effects 0.000 claims description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 239000000908 ammonium hydroxide Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical group [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 8
- -1 silicon Alkane Chemical class 0.000 description 6
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention belongs to LED encapsulation material technical field, and in particular to a kind of LED encapsulation organic siliconresin and preparation method thereof, the LED encapsulation organic siliconresins are made up of following parts by weight：5 10 parts of methyl trichlorosilane, 45 90 parts of phenyl trichlorosilane, 15 30 parts of methylvinyldichlorosilane, 10 15 parts of dimethoxydiphenylsilane, 38 parts of catalyst, 35 parts of absolute ethyl alcohol, 90 100 parts of dimethylbenzene, 10 20 parts of n-butanol, 20 300 parts of distilled water, 26 parts of crosslinking and curing agent, 2 10 parts of nanometer diamond alkene.The invention mechanical strength is good, and thermal conductivity is good, and stability is high.
Description
Technical field
The invention belongs to LED encapsulation material technical field, and in particular to LED encapsulation organic siliconresin and its preparation side
Method.
Background technology
Light emitting diode（LED）Have the advantages that energy consumption is low, environmentally friendly due to it, durable be widely used.LED encapsulation is right
The encapsulation of luminescence chip, is to load encapsulating material to be placed with the device of electronic component and circuit, and its effect is sealing protection
Heat, reduction chip and air that moisture, the normal use of protection device in LED chip, isolation air, discharge chip are produced
In refractive index difference, isolation influence to chip assembly of extraneous vibration etc..In encapsulation process, because LED is in the course of work
In the electric energy of only 30%-40% be converted into the electric energy of light residue 60%-70% and be converted into heat energy, if the heat of chip internal can not
Pass in time, the attenuating of LED luminous efficiencies and luminous intensity can be caused, while the electrical part life-span can also shorten, therefore LED
Influence of the selection of encapsulating material to its performance is very crucial.
Conventional encapsulating material has epoxy resin, organic siliconresin, modified silicon rubber etc., wherein organic siliconresin phase at present
, refractive index higher than the heat-resisting of other encapsulating materials, ultraviolet-resistant aging, light transmittance is high, but organic siliconresin has machinery
The shortcomings of intensity is relatively low, heat conductivility is poor, stability is poor, it is therefore desirable to further to improve.
The content of the invention
Good it is an object of the invention to provide mechanical strength, thermal conductivity is good, a kind of stability LED encapsulation organosilicon high
Resin.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of LED encapsulation organic siliconresin, is made up of following parts by weight：Methyl trichlorosilane 5-10 parts, phenyl trichlorine silicon
Alkane 45-90 parts, methylvinyldichlorosilane 15-30 parts, dimethoxydiphenylsilane 10-15 parts, catalyst 3-8 parts, nothing
Water-ethanol 3-5 parts, dimethylbenzene 90-100 parts, n-butanol 10-20 parts, distilled water 20-300 parts, crosslinking and curing agent 2-6 parts, nanometer
2-10 parts of diamond alkene.
Further, described catalyst is TMAH.
Further, described nanometer diamond alkene is modified nanometer diamond alkene, and its method of modifying is as follows：
A. ultrasonic wave alkali cleaning：Nanometer diamond alkene is put into stirring and washing, ultrasonic frequency in the supersonic wave cleaning machine equipped with alkali lye
It is 35-40KHz, alkali lye is the NaOH solution of 10-12wt%, and alkali cleaning temperature is 50-60 DEG C, and mixing speed is 35-40rpm, cleaning
20-30min；
B. ultrasonic wave water washing：Nanometer diamond alkene after alkali cleaning is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 30-40KHz, mixing speed 10-20rpm, stirring and washing 15-20min, measures supernatant liquor pH value,
Cleaning is until pH=7 repeatedly；
C. acid-wash activation：Nanometer diamond alkene after being washed in step b adds stirring and washing in pickle, and described pickle is
The salpeter solution of 25-30wt%, 25-30 DEG C of pickling temperature, mixing speed is 30-35rpm, and mixing time is 15-20min；
D. ultrasonic wave water washing：Nanometer diamond alkene after pickling is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 30-35KHz, and mixing speed is 10-20rpm, stirring and washing 15-20min, takes supernatant liquor measurement
PH value, cleaning after pH=7 until dry repeatedly；
E. stirred in the nanometer diamond alkene in step d being added into the absolute ethyl alcohol containing silane coupler, described absolute ethyl alcohol
Middle silane coupler mass concentration is 2%-6%, and whipping temp is 60-65 DEG C, and mixing time is 2-3h, is then filtered dry
It is dry, obtain modified nanometer diamond alkene.
Further, the silane coupler of step e is KH550 in described nanometer diamond alkene method of modifying, and the KH550 is used
Amount is 2.5%-4.5% with the ratio of the consumption of nanometer diamond alkene.
Further, described nanometer diamond alkene grain size proportion is 50nm ︰ 100nm ︰ 200nm=(1-2) ︰ (2-3) ︰ (4-
5)。
Further, a kind of preparation method of described LED encapsulation organic siliconresin, comprises the steps of：
（1）Methyl trichlorosilane, phenyl trichlorosilane and methylvinyldichlorosilane are mixed in raw material 60% dimethylbenzene
In solution, chlorosilane solution is obtained；
（2）Stirred during remaining 40% dimethylbenzene in absolute ethyl alcohol, raw material and n-butanol are added into distilled water, by step（1）
Middle chlorosilane solution passes through to be added dropwise in the mixed solution that stirs, and the reaction time is 2-2.5h, and reaction temperature is 70-
80℃；
（3）By step（2）In the layering of reacted solution left standstill, take upper strata organic solvent, use 65-70 DEG C of deionized water water
Filtered after washing upper solution to neutrality, distill out organic solvent；
（4）The organic solvent for obtaining will be distilled and be heated to 70-80 DEG C, dimethoxydiphenylsilane is added while stirring, stirred
1-2h, then cools down, vacuum distillation, obtains organic siliconresin aggressiveness；
（5）By step（4）In organic siliconresin aggressiveness add catalyst while stirring, reaction temperature is 150-160 DEG C, stirring
Vacuum distillation obtains organic siliconresin matrix after 4-5h；
（6）Nanometer diamond alkene is mixed with organic siliconresin matrix, adds crosslinking and curing agent and catalyst to stir, then with
5 DEG C/min speed is warming up to 50-60 DEG C of solidification 2-2.5h, then is warming up to 150-160 DEG C of solidification 5-6h with 8 DEG C/min speed, obtains
Finished product.
Compared with prior art, technique effect of the invention is：
Because modified nanometer diamond alkene dispersion force is strong, finely dispersed heat conduction can be formed in addition organic resin based composites
Network, reduces the thermal resistance of composite, and making the organic siliconresin of obtained LED encapsulation has high thermal conductivity, also reduces organic
The thermal stress that silicones causes because thermal expansion is uneven, increases the thermal diffusivity of the LED materials of encapsulation, further, since receiving
Rice diamond alkene has extraordinary insulating properties, it is largely ensure that its security appliance performance and service life, this hair
Bright also to have preferable mechanical strength, ultraviolet light resistant, light transmittance are high, heat-resist, can be sealed as a kind of great power LED
Package material.
Brief description of the drawings
Fig. 1 be embodiment 1 in KH550 consumptions led with organic siliconresin with LED encapsulation with the ratio of nanometer diamond alkene consumption
Relation schematic diagram between heating rate；
Fig. 2 is that the relation between the addition of nanometer diamond alkene in embodiment 1 and LED encapsulation organic siliconresin thermal conductivitys is illustrated
Figure.
Specific embodiment
Embodiment 1：
A kind of LED encapsulation organic siliconresin, is made up of following parts by weight：5 parts of methyl trichlorosilane, phenyl trichlorosilane 45
Part, 15 parts of methylvinyldichlorosilane, 10 parts of dimethoxydiphenylsilane, 3 parts of catalyst, 3 parts of absolute ethyl alcohol, dimethylbenzene
90 parts, 10 parts of n-butanol, 20 parts of distilled water, 2 parts of crosslinking and curing agent, 2 parts of nanometer diamond alkene.
Described nanometer diamond alkene is modified nanometer diamond alkene, and its method of modifying is as follows：
A. ultrasonic wave alkali cleaning：Nanometer diamond alkene is put into stirring and washing, ultrasonic frequency in the supersonic wave cleaning machine equipped with alkali lye
It is 35KHz, alkali lye is the NaOH solution of 10wt%, and alkali cleaning temperature is 50 DEG C, and mixing speed is 35rpm, cleans 20min；
B. ultrasonic wave water washing：Nanometer diamond alkene after alkali cleaning is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 30KHz, mixing speed 10rpm, stirring and washing 15min, measures supernatant liquor pH value, is cleaned repeatedly
Until pH=7；
C. acid-wash activation：Nanometer diamond alkene after being washed in step b adds stirring and washing in pickle, and described pickle is
The salpeter solution of 25wt%, 25 DEG C of pickling temperature, mixing speed is 30rpm, and mixing time is 15min；
D. ultrasonic wave water washing：Nanometer diamond alkene after pickling is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 30KHz, and mixing speed is 10rpm, stirring and washing 15min, takes supernatant liquor pH value determination, repeatedly
Cleaning after pH=7 until dry.
E. stirred in the nanometer diamond alkene in step d being added into the absolute ethyl alcohol containing KH550, described absolute ethyl alcohol
Middle silane coupler mass concentration is 2%, and whipping temp is 60 DEG C, and mixing time is 2h, then carries out filtration drying, obtains modified
Nanometer diamond alkene, the ratio of the consumption of the KH550 consumptions and nanometer diamond alkene is 2.5%%.
Further, a kind of preparation method of described LED encapsulation organic siliconresin, comprises the steps of：
（1）Methyl trichlorosilane, phenyl trichlorosilane and methylvinyldichlorosilane are mixed in raw material 60% dimethylbenzene
In solution, chlorosilane solution is obtained；
（2）Stirred during remaining 40% dimethylbenzene in absolute ethyl alcohol, raw material and n-butanol are added into distilled water, by step（1）
By being added dropwise in mixed solution, the reaction time is 2h to middle chlorosilane solution, and reaction temperature is 70 DEG C；
（3）By step（2）In the layering of reacted solution left standstill, take upper strata organic solvent, use 65 DEG C of deionized waters to wash
Filtered after upper solution to neutrality, distill out organic solvent；
（4）The organic solvent for obtaining will be distilled and is heated to 70 DEG C, dimethoxydiphenylsilane is added while stirring, stir 1h,
Then cool down, vacuum distillation, obtain organic siliconresin aggressiveness；
（5）By step（4）In organic siliconresin aggressiveness add TMAH while stirring, reaction temperature is 150 DEG C,
Vacuum distillation obtains organic siliconresin matrix after stirring 4h；
（6）Nanometer diamond alkene is mixed with organic siliconresin matrix, aminopropyl triethoxysilane and tetramethyl hydroxide is added
Ammonium stirs, and is then warming up to 50 DEG C of solidification 2-2.5h with 5 DEG C/min speed, then be warming up to 150 DEG C admittedly with 8 DEG C/min speed
Change 5-6h, obtain finished product.
Embodiment 2：
A kind of LED encapsulation organic siliconresin, is made up of following parts by weight：7.5 parts of methyl trichlorosilane, phenyl trichlorosilane
67.5 parts, 22.5 parts of methylvinyldichlorosilane, 12.5 parts of dimethoxydiphenylsilane, 5.5 parts of catalyst, absolute ethyl alcohol
4 parts, 95 parts of dimethylbenzene, 15 parts of n-butanol, 160 parts of distilled water, 4 parts of crosslinking and curing agent, 6 parts of nanometer diamond alkene.
Described nanometer diamond alkene is modified nanometer diamond alkene, and its method of modifying is as follows：
A. ultrasonic wave alkali cleaning：Nanometer diamond alkene is put into stirring and washing, ultrasonic frequency in the supersonic wave cleaning machine equipped with alkali lye
It is 37.5KHz, alkali lye is the NaOH solution of 11wt%, and alkali cleaning temperature is 55 DEG C, and mixing speed is 37rpm, cleans 25min；
B. ultrasonic wave water washing：Nanometer diamond alkene after alkali cleaning is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 35KHz, mixing speed 15rpm, stirring and washing 17min, measures supernatant liquor pH value, is cleaned repeatedly
Until pH=7；
C. acid-wash activation：Nanometer diamond alkene after being washed in step b adds stirring and washing in pickle, and described pickle is
The salpeter solution of 27wt%, 27 DEG C of pickling temperature, mixing speed is 32rpm, and mixing time is 17min；
D. ultrasonic wave water washing：Nanometer diamond alkene after pickling is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 32KHz, and mixing speed is 15rpm, stirring and washing 17min, takes supernatant liquor pH value determination, repeatedly
Cleaning after pH=7 until dry；
E. stirred in the nanometer diamond alkene in step d being added into the absolute ethyl alcohol containing KH550, silicon in described absolute ethyl alcohol
Alkane coupling agent mass concentration is 4%, and whipping temp is 62 DEG C, and mixing time is 2.5h, then carries out filtration drying, obtains modified
Nanometer diamond alkene, the KH550 consumptions are 2.5%3.5% with the ratio of the consumption of nanometer diamond alkene.
A kind of preparation method of described LED encapsulation organic siliconresin, comprises the steps of：
（1）Methyl trichlorosilane, phenyl trichlorosilane and methylvinyldichlorosilane are mixed in raw material 60% dimethylbenzene
In solution, chlorosilane solution is obtained；
（2）Stirred during remaining 40% dimethylbenzene in absolute ethyl alcohol, raw material and n-butanol are added into distilled water, by step（1）
By being added dropwise in mixed solution, the reaction time is 2.25h to middle chlorosilane solution, and reaction temperature is 75 DEG C；
（3）By step（2）In the layering of reacted solution left standstill, take upper strata organic solvent, use 67 DEG C of deionized waters to wash
Filtered after upper solution to neutrality, distill out organic solvent；
（4）The organic solvent for obtaining will be distilled and be heated to 75 DEG C, dimethoxydiphenylsilane is added while stirring, stirred
1.5h, then cools down, vacuum distillation, obtains organic siliconresin aggressiveness；
（5）By step（4）In organic siliconresin aggressiveness add TMAH while stirring, reaction temperature is 155 DEG C,
Vacuum distillation obtains organic siliconresin matrix after stirring 4-5h；
（6）Nanometer diamond alkene is mixed with organic siliconresin matrix, aminopropyl triethoxysilane and tetramethyl hydroxide is added
Ammonium stirs, and is then warming up to 55 DEG C of solidification 2.25h with 5 DEG C/min speed, then be warming up to 155 DEG C admittedly with 8 DEG C/min speed
Change 5.5h, obtain finished product.
Embodiment 3
A kind of LED encapsulation organic siliconresin, is made up of following parts by weight：10 parts of methyl trichlorosilane, phenyl trichlorosilane
90 parts, 30 parts of methylvinyldichlorosilane, 15 parts of dimethoxydiphenylsilane, 8 parts of catalyst, 5 parts of absolute ethyl alcohol, diformazan
100 parts of benzene, 20 parts of n-butanol, 300 parts of distilled water, 6 parts of crosslinking and curing agent, 10 parts of nanometer diamond alkene.
Described nanometer diamond alkene is modified nanometer diamond alkene, and its method of modifying is as follows：
A. ultrasonic wave alkali cleaning：Nanometer diamond alkene is put into stirring and washing, ultrasonic frequency in the supersonic wave cleaning machine equipped with alkali lye
It is 40KHz, alkali lye is the NaOH solution of 12wt%, and alkali cleaning temperature is 60 DEG C, and mixing speed is 40rpm, cleans 30min；
B. ultrasonic wave water washing：Nanometer diamond alkene after alkali cleaning is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 40KHz, mixing speed 20rpm, stirring and washing 20min, measures supernatant liquor pH value, is cleaned repeatedly
Until pH=7；
C. acid-wash activation：Nanometer diamond alkene after being washed in step b adds stirring and washing in pickle, and described pickle is
The salpeter solution of 30wt%, 30 DEG C of pickling temperature, mixing speed is 35rpm, and mixing time is 20min；
D. ultrasonic wave water washing：Nanometer diamond alkene after pickling is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 35KHz, and mixing speed is 20rpm, stirring and washing 20min, takes supernatant liquor pH value determination, repeatedly
Cleaning after pH=7 until dry；
E. stirred in the nanometer diamond alkene in step d being added into the absolute ethyl alcohol containing KH550, silicon in described absolute ethyl alcohol
Alkane coupling agent mass concentration is 6%, and whipping temp is 65 DEG C, and mixing time is 3h, then carries out filtration drying, obtains modified receiving
Rice diamond alkene, the KH550 consumptions are 4.5% with the ratio of the consumption of nanometer diamond alkene.
A kind of preparation method of described LED encapsulation organic siliconresin, comprises the steps of：
（1）Methyl trichlorosilane, phenyl trichlorosilane and methylvinyldichlorosilane are mixed in raw material 60% dimethylbenzene
In solution, chlorosilane solution is obtained；
（2）Stirred during remaining 40% dimethylbenzene in absolute ethyl alcohol, raw material and n-butanol are added into distilled water, by step（1）
By being added dropwise in mixed solution, the reaction time is 2.5h to middle chlorosilane solution, and reaction temperature is 80 DEG C；
（3）By step（2）In the layering of reacted solution left standstill, take upper strata organic solvent, use 70 DEG C of deionized waters to wash
Filtered after upper solution to neutrality, distill out organic solvent；
（4）The organic solvent for obtaining will be distilled and is heated to 80 DEG C, dimethoxydiphenylsilane is added while stirring, stir 2h,
Then cool down, vacuum distillation, obtain organic siliconresin aggressiveness；
（5）By step（4）In organic siliconresin aggressiveness add TMAH while stirring, reaction temperature is 160 DEG C,
Vacuum distillation obtains organic siliconresin matrix after stirring 5h；
（6）Nanometer diamond alkene is mixed with organic siliconresin matrix, aminopropyl triethoxysilane and tetramethyl hydroxide is added
Ammonium stirs, and is then warming up to 60 DEG C of solidification 2.5h with 5 DEG C/min speed, then be warming up to 160 DEG C of solidifications with 8 DEG C/min speed
6h, obtains finished product.
Test example 1：
A kind of LED encapsulation organic siliconresin of the present embodiment 1, wherein nanometer diamond alkene are modified nanometer diamond alkene, the nanometer
In the step of diamond alkene method of modifying e, the ratio with described KH550 consumptions and nanometer diamond alkene consumption uses heat as variable
Stream method to being 0-10% in the variable between prepared LED encapsulation detected with the thermal conductivity of organic siliconresin, such as Fig. 1 institutes
Show, add the thermal conductivity of the LED encapsulation organic siliconresins prepared by modified nanometer diamond alkene relative to being not added with being modified
The thermal conductivity of the LED encapsulation organic siliconresins prepared by nanometer diamond alkene afterwards is good, when KH550 consumptions reach nanometer diamond alkene
During the 2.5-4.5% of consumption, the thermal conductivity of LED encapsulation organic siliconresins is preferable, when KH550 consumptions and nanometer diamond alkene consumption
Ratio when being more than 4.5%, modified nanometer diamond alkene produces thicker coupling agent film with organic siliconresin matrix, makes it
Thermal conductivity reduction, therefore, when KH550 consumptions and nanometer diamond alkene consumption are between 2.5%-4.5%, the LED encapsulation that it is made
Thermal conductivity with organic siliconresin is more suitable.
Test example 2：
Using the addition amount of the nanometer diamond alkene being modified in a kind of LED encapsulation organic siliconresin in embodiment 1 as variable, make
LED encapsulation organic siliconresin is detected with heat flow method, as shown in Fig. 2
The thermal conductivity of prepared LED encapsulation organic siliconresins is relative after addition nanometer diamond alkene is not added with nanometer diamond alkene
Thermal conductivity increases, and with the increase of addition, its thermal conductivity is constantly raised, and can all be caused because nano-particle is excessively added
The mechanical property reduction of composite, so the addition of nanometer diamond alkene is more suitable between 2-10.
Claims (6)
1. a kind of LED encapsulation organic siliconresin, it is characterised in that be made up of following parts by weight：Methyl trichlorosilane 5-10
Part, phenyl trichlorosilane 45-90 parts, methylvinyldichlorosilane 15-30 parts, dimethoxydiphenylsilane 10-15 parts, urge
Agent 3-8 parts, absolute ethyl alcohol 3-5 parts, dimethylbenzene 90-100 parts, n-butanol 10-20 parts, distilled water 20-300 parts, crosslinking curing
Agent 2-6 parts, 2-10 parts of nanometer diamond alkene.
2. a kind of LED encapsulation organic siliconresin according to claim 1, it is characterised in that described catalyst is four
Ammonium hydroxide.
3. LED encapsulation organic siliconresin according to claim 2, it is characterised in that described nanometer diamond alkene is to change
The nanometer diamond alkene of property, its method of modifying is as follows：
A. ultrasonic wave alkali cleaning：Nanometer diamond alkene is put into stirring and washing, ultrasonic frequency in the supersonic wave cleaning machine equipped with alkali lye
It is 35-40KHz, alkali lye is the NaOH solution of 10-12wt%, and alkali cleaning temperature is 50-60 DEG C, and mixing speed is 35-40rpm, cleaning
20-30min；
B. ultrasonic wave water washing：Nanometer diamond alkene after alkali cleaning is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 30-40KHz, mixing speed 10-20rpm, stirring and washing 15-20min, measures supernatant liquor pH value,
Cleaning is until pH=7 repeatedly；
C. acid-wash activation：Nanometer diamond alkene after being washed in step b adds stirring and washing in pickle, and described pickle is
The salpeter solution of 25-30wt%, 25-30 DEG C of pickling temperature, mixing speed is 30-35rpm, and mixing time is 15-20min；
D. ultrasonic wave water washing：Nanometer diamond alkene after pickling is put into stirring at normal temperature in the supersonic wave cleaning machine equipped with deionized water
Cleaning, ultrasonic frequency is 30-35KHz, and mixing speed is 10-20rpm, stirring and washing 15-20min, takes supernatant liquor measurement
PH value, cleaning after pH=7 until dry repeatedly；
E. stirred in the nanometer diamond alkene in step d being added into the absolute ethyl alcohol containing silane coupler, described absolute ethyl alcohol
Middle silane coupler mass concentration is 2%-6%, and whipping temp is 60-65 DEG C, and mixing time is 2-3h, is then filtered dry
It is dry, obtain modified nanometer diamond alkene.
4. a kind of LED encapsulation organic siliconresin according to claim 3, it is characterised in that described nanometer diamond alkene
The silane coupler of step e is KH550 in method of modifying, and the KH550 consumptions are 2.5%- with the ratio of the consumption of nanometer diamond alkene
4.5%。
5. a kind of LED encapsulation organic siliconresin according to claim 4, it is characterised in that described nanometer diamond alkene
Grain size proportion is 50nm ︰ 100nm ︰ 200nm=(1-2) ︰ (2-3) ︰ (4-5).
6. the preparation method of a kind of LED encapsulation organic siliconresin according to claim 5, it is characterised in that by following
Step is constituted：
（1）Methyl trichlorosilane, phenyl trichlorosilane and methylvinyldichlorosilane are mixed in raw material 60% dimethylbenzene
In solution, chlorosilane solution is obtained；
（2）Stirred during remaining 40% dimethylbenzene in absolute ethyl alcohol, raw material and n-butanol are added into distilled water, by step（1）
Middle chlorosilane solution passes through to be added dropwise in the mixed solution that stirs, and the reaction time is 2-2.5h, and reaction temperature is 70-
80℃；
（3）By step（2）In the layering of reacted solution left standstill, take upper strata organic solvent, use 65-70 DEG C of deionized water water
Filtered after washing upper solution to neutrality, distill out organic solvent；
（4）The organic solvent for obtaining will be distilled and be heated to 70-80 DEG C, dimethoxydiphenylsilane is added while stirring, stirred
1-2h, then cools down, vacuum distillation, obtains organic siliconresin aggressiveness；
（5）By step（4）In organic siliconresin aggressiveness add catalyst while stirring, reaction temperature is 150-160 DEG C, stirring
Vacuum distillation obtains organic siliconresin matrix after 4-5h；
（6）Nanometer diamond alkene is mixed with organic siliconresin matrix, adds crosslinking and curing agent and catalyst to stir, then with
5 DEG C/min speed is warming up to 50-60 DEG C of solidification 2-2.5h, then is warming up to 150-160 DEG C of solidification 5-6h with 8 DEG C/min speed, obtains
Finished product.
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Application publication date: 20170613 |