CN110183661A - A kind of high heat resistance, the preparation method of High-heat-conductiviinsulation insulation material - Google Patents
A kind of high heat resistance, the preparation method of High-heat-conductiviinsulation insulation material Download PDFInfo
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- CN110183661A CN110183661A CN201910494435.9A CN201910494435A CN110183661A CN 110183661 A CN110183661 A CN 110183661A CN 201910494435 A CN201910494435 A CN 201910494435A CN 110183661 A CN110183661 A CN 110183661A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000012774 insulation material Substances 0.000 title claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 38
- 235000019441 ethanol Nutrition 0.000 claims abstract description 33
- 239000011810 insulating material Substances 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 7
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000004809 Teflon Substances 0.000 claims abstract description 4
- 229920006362 Teflon® Polymers 0.000 claims abstract description 4
- 238000006482 condensation reaction Methods 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 6
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- -1 methyltriethoxy silane Alkane Chemical class 0.000 claims description 3
- 238000003475 lamination Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 abstract description 12
- 239000002904 solvent Substances 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000004411 aluminium Substances 0.000 description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000006053 organic reaction Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 229910017083 AlN Inorganic materials 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- ZXPDYFSTVHQQOI-UHFFFAOYSA-N diethoxysilane Chemical compound CCO[SiH2]OCC ZXPDYFSTVHQQOI-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000001905 inorganic group Chemical group 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C08G77/06—Preparatory processes
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a kind of high heat resistance, the preparation method of High-heat-conductiviinsulation insulation material, includes the following steps: that (1) mixes the Organosilicon Alcohol in Organic solution 5-20 parts by weight that solid content is 25%-30% with 30 parts by weight of alumina powder, condensation reaction occurs；(2) slurry is injected in Teflon mould, volatilization removes water and ethyl alcohol equal solvent, while making part of hydroxyl that polycondensation reaction occur；(3) polycondensation product is laminated using vacuum laminator, obtains insulating materials.When Organosilicon Alcohol in Organic solution of the invention is mixed with alumina powder, because polarity is close small with steric hindrance, Organosilicon Alcohol in Organic can sufficiently soak alumina powder, the uniformity of insulating materials composition and performance can significantly improve, the interface resistance being substantially reduced between alumina powder and organic matrix, to obtain the insulating materials of high thermal conductivity, be conducive to aluminum-based copper-clad plate in the popularization and use of high field of radiating.
Description
Technical field
The present invention relates to aluminum-based copper-clad plate technical field, more particularly to a kind of high heat resistance, High-heat-conductiviinsulation insulation material
Preparation method.
Background technique
In field of LED illumination, the heat resistance and heating conduction of substrate are to illumination light effect, device service life and reliability
All have highly important meaning.Small, thin, the light development trend of illuminating device proposes higher and higher want to substrate heat dissipation
It asks, therefore the heat-radiating substrate of high heat resistance, high thermal conductivity, becomes focus concerned by people.
Aluminum-based copper-clad plate is made of copper foil, insulating layer and aluminium sheet.After insulating layer mainly uses glass-fiber-fabric epoxy resin-impregnated
It toasts, this insulating materials excellent insulating property is easy to process, but the lower (0.1-0.2Wm of thermal coefficient-1·K-1),
It is not able to satisfy the needs of high heat dissipation product.
Patent CN105704911A (a kind of preparation method on high thermal conductivity aluminum matrix printed line road) is reported with epoxy resin, phenolic aldehyde tree
Rouge is basic resin, and using aluminium oxide, aluminium nitride, boron nitride as heat filling, covers after being stirred and is pressed in formation height on aluminium sheet
The thermal coefficient of thermally conductive aluminum substrate, insulating layer reaches 2.2Wm-1·K-1, dielectric strength reaches 30-42kVmm-1.But nitrogen
Change aluminium, boron nitride higher cost, using being restricted.
The performance of insulating materials is extremely important to high-capacity LED.Resin used in insulating materials is mostly asphalt mixtures modified by epoxy resin at present
Rouge haves the defects that temperature tolerance is poor, is unable to satisfy the heatproof requirement of high-power product.Meanwhile epoxy resin and inorganic particle
Poor compatibility, cause two-phase interface thermal resistance big, seriously affect the thermal coefficient of composite material.In addition, addition aluminium nitride, nitridation
Boron will lead to insulating materials, and increased production cost.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides the preparation sides of a kind of high heat resistance, High-heat-conductiviinsulation insulation material
Method.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of high heat resistance, the preparation method of High-heat-conductiviinsulation insulation material, include the following steps:
(1) the Organosilicon Alcohol in Organic solution 5-20 parts by weight that solid content is 25%-30% are mixed with 30 parts by weight of alumina powder
It closes, then by heating, makes-the OH on the alumina powder surface in slurry and the-OH in silanol that condensation reaction occur, steam simultaneously
Send out part water and ethyl alcohol；
(2) slurry is injected in polytetrafluoroethylene (PTFE) (PTFE) mold, heats 8-12h at 60-100 DEG C to volatilize and removes water
With ethyl alcohol equal solvent, while make part of hydroxyl occur polycondensation reaction；
(3) finally polycondensation product is laminated using vacuum laminator, obtains the sheet type insulation of high heat resistance, high thermal conductivity
Material.
Preferably, in above-mentioned preparation method, the alumina powder is spherical shape, partial size is 0.5 μm, 2.5 μm,
One or more of 5 μm, 10 μm.
Preferably, in above-mentioned preparation method, the lamination are as follows: 160 DEG C, 10MPa, 5min.
Preferably, the Organosilicon Alcohol in Organic solution is by methyltriethoxysilane, diformazan in above-mentioned preparation method
Base diethoxy silane and phenyltrimethoxysila,e are made.Its inorganic group content is higher, and temperature tolerance is excellent, and with aluminium sheet
Adhesive force is good.
Preferably, above-mentioned preparation method the following steps are included:
(1) by methyltriethoxysilane, dimethyl diethoxysilane and phenyltrimethoxysila,e and deionization
After water mixing, 1.5h is stirred at 60 DEG C；Organosilan hydrolyzes, and obtains the Organosilicon Alcohol in Organic solution that solid content is 25%-30%；
(2) 30 parts of composite alumina powders are added in Organosilicon Alcohol in Organic solution, 0.5h is stirred under room temperature, then by slurry
60 DEG C are heated to, is condensed Organosilicon Alcohol in Organic with alumina powder surface hydroxyl, while part water and ethyl alcohol volatilization, is had
There is the slurry of certain viscosity；
(3) slurry is injected into Teflon mould, 8h is toasted at 60 DEG C, 2h is toasted at 100 DEG C, obtains semi-solid preparation
Sheet type insulating materials, sheet thickness control between 3-5mm；
(4) half-and-half cured insulating materials closes heating later, keeps it cold with furnace in 160 DEG C, 10MPa laminated 5min
But, high heat resistance, High-heat-conductiviinsulation insulation material are obtained.
Preferably, 30 parts of composite alumina powders are by 21 parts of 10 μm of aluminium oxide in above-mentioned preparation method
Powder and 9 parts of 0.5 μm of alumina powder compositions.
Compared with prior art, the invention has the following beneficial effects:
(1) using the organic siliconresin of semi-solid preparation as link stuff, the heat resistance of insulating materials is obviously improved；
(2) when Organosilicon Alcohol in Organic solution is mixed with alumina powder, because polarity is close small with steric hindrance, Organosilicon Alcohol in Organic can
Sufficiently wetting alumina powder, the uniformity of insulating materials composition and performance can significantly improve.
(3) condensation reaction occurs for the hydroxyl on the short chain of hydroxyl Yu Organosilicon Alcohol in Organic on alumina powder surface, can obviously reduce
Interface resistance between alumina powder and organic matrix, to obtain the insulating materials of high thermal conductivity.
(4) alumina powder thermal coefficient is larger, and chemical property is stablized, and from a wealth of sources, price is lower, is conducive to the technology
Popularization and use.
Specific embodiment:
With example, the present invention is further illustrated below, but example cannot illustrate the limit to the scope of the present invention
System, person skilled in art can carry out nonessential modifications and adaptations to example.
Embodiment 1:
(1) weighed respectively by mass parts 47.5 parts of methyltriethoxysilane, 29.6 parts of dimethyl diethoxysilanes,
13.2 parts of phenyltrimethoxysila,es and 40 parts of deionized waters stir 1.5h at 60 DEG C, it is molten to form homogeneous and transparent Organosilicon Alcohol in Organic
Liquid.
(2) 17.5 parts of Organosilicon Alcohol in Organic solution in (1), the composite alumina powder of 30 parts of drying, wherein 10 μm of oxidations are taken
It 21 parts of aluminium powder body, 0.5 μm 9 parts of alumina powder, is stirred at 60 DEG C, contracts between alumina powder and Organosilicon Alcohol in Organic
Reaction, while evaporation section solvent are closed, slurry is obtained；
(3) slurry is injected into PTFE mold (control is with a thickness of 3-5mm), 8h, 100 DEG C of baking 2h is toasted at 60 DEG C,
And in 160 DEG C, 10MPa laminated 5min, stops heating, obtain insulating materials after furnace cooling.
Embodiment 2:
(1) weighed respectively by mass parts 47.5 parts of methyltriethoxysilane, 29.6 parts of dimethyl diethoxysilanes,
13.2 parts of phenyltrimethoxysila,es and 40 parts of deionized waters stir 1.5h at 60 DEG C, it is molten to form homogeneous and transparent Organosilicon Alcohol in Organic
Liquid.
(2) 7.65 parts of Organosilicon Alcohol in Organic solution in (1), the composite alumina powder of 30 parts of drying, wherein 10 μm of oxidations are taken
It 21 parts of aluminium powder body, 0.5 μm 9 parts of alumina powder, is stirred at 60 DEG C, contracts between alumina powder and Organosilicon Alcohol in Organic
Reaction, while evaporation section solvent are closed, slurry is obtained；
(3) slurry is injected into PTFE mold (control is with a thickness of 3-5mm), 8h, 100 DEG C of baking 2h is toasted at 60 DEG C,
And in 160 DEG C, 10MPa laminated 5min, stops heating, obtain insulating materials after furnace cooling.
Embodiment 3:
(1) weighed respectively by mass parts 47.5 parts of methyltriethoxysilane, 29.6 parts of dimethyl diethoxysilanes,
13.2 parts of phenyltrimethoxysila,es and 40 parts of deionized waters stir 1.5h at 60 DEG C, it is molten to form homogeneous and transparent Organosilicon Alcohol in Organic
Liquid.
(2) 10.8 parts of Organosilicon Alcohol in Organic solution in (1), the composite alumina powder of 30 parts of drying, wherein 10 μm of oxidations are taken
It 21 parts of aluminium powder body, 0.5 μm 9 parts of alumina powder, is stirred at 60 DEG C, is condensed between alumina powder and Organosilicon Alcohol in Organic
Reaction, while evaporation section solvent, obtain slurry；
(3) slurry is injected into PTFE mold (control is with a thickness of 3-5mm), 8h, 100 DEG C of baking 2h is toasted at 60 DEG C,
And in 160 DEG C, 10MPa laminated 5min, stops heating, obtain insulating materials after furnace cooling.
Test result:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Organosilicon Alcohol in Organic solution | 17.5 parts | 7.65 part | 10.8 parts |
| Alumina powder | 30 parts | 30 parts | 30 parts |
| Thermal coefficient | 1.73W·m-1·K-1 | 2.97W·m-1·K-1 | 2.49W·m-1·K-1 |
| Breakdown strength | 50kV·mm-1 | 22kV·mm-1 | 28kV·mm-1 |
| Thermal decomposition temperature (heat loss amount 5%) | 572℃ | >800℃ | >800℃ |
Claims (6)
1. a kind of high heat resistance, the preparation method of High-heat-conductiviinsulation insulation material, it is characterised in that include the following steps:
(1) the Organosilicon Alcohol in Organic solution 5-20 parts by weight that solid content is 25%-30% are mixed with 30 parts by weight of alumina powder, then
By heating, make-the OH on the alumina powder surface in slurry and the-OH in silanol that condensation reaction, while evaporation section occur
Water and ethyl alcohol；
(2) slurry is injected in Teflon mould, heats 8-12h at 60-100 DEG C to volatilize and remove water and ethyl alcohol, together
When make part of hydroxyl occur polycondensation reaction；
(3) finally polycondensation product is laminated using vacuum laminator, obtains high heat resistance, the sheet type insulation material of high thermal conductivity
Material.
2. preparation method as described in claim 1, which is characterized in that the alumina powder be spherical shape, partial size be 0.5 μm,
One or more of 2.5 μm, 5 μm, 10 μm.
3. preparation method as described in claim 1, which is characterized in that the Organosilicon Alcohol in Organic solution is by methyltriethoxy silane
Alkane, dimethyl diethoxysilane and phenyltrimethoxysila,e are made.
4. preparation method as described in claim 1, which is characterized in that the lamination are as follows: 160 DEG C, 10MPa, 5min.
5. preparation method as described in claim 1, which comprises the following steps:
(1) methyltriethoxysilane, dimethyl diethoxysilane and phenyltrimethoxysila,e and deionized water are mixed
After conjunction, 1.5h is stirred at 60 DEG C；Organosilan hydrolyzes, and obtains the Organosilicon Alcohol in Organic solution that solid content is 25%-30%；
(2) composite alumina powder is added in Organosilicon Alcohol in Organic solution, 0.5h is stirred under room temperature, slurry is then heated to 60
DEG C, it is condensed Organosilicon Alcohol in Organic with alumina powder surface hydroxyl, while part water and ethyl alcohol volatilization, obtains having certain glutinous
The slurry of degree；
(3) slurry is injected into Teflon mould, 8h is toasted at 60 DEG C, toasts 2h at 100 DEG C, obtains the thin of semi-solid preparation
Chip insulating materials, sheet thickness control between 3-5mm；
(4) half-and-half cured insulating materials closes heating later, makes its furnace cooling in 160 DEG C, 10MPa laminated 5min,
Obtain high heat resistance, High-heat-conductiviinsulation insulation material.
6. preparation method as claimed in claim 5, which is characterized in that the composite alumina powder is by 21 parts of 10 μm of aluminium oxide
Powder and 9 parts of 0.5 μm of alumina powder compositions.
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| CN201910494435.9A CN110183661A (en) | 2019-06-10 | 2019-06-10 | A kind of high heat resistance, the preparation method of High-heat-conductiviinsulation insulation material |
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Application publication date: 20190830 |