CN117089318B - Organic silicon die-bonding adhesive and preparation method and application thereof - Google Patents
Organic silicon die-bonding adhesive and preparation method and application thereof Download PDFInfo
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- CN117089318B CN117089318B CN202310919978.7A CN202310919978A CN117089318B CN 117089318 B CN117089318 B CN 117089318B CN 202310919978 A CN202310919978 A CN 202310919978A CN 117089318 B CN117089318 B CN 117089318B
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- die
- silicone resin
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- organic silicon
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- 239000000853 adhesive Substances 0.000 title claims abstract description 74
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 74
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 39
- 239000010703 silicon Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- -1 methyl propenyl Chemical group 0.000 claims abstract description 56
- 229920002050 silicone resin Polymers 0.000 claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000006229 carbon black Substances 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 11
- 125000005395 methacrylic acid group Chemical group 0.000 claims abstract description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 26
- 229920005989 resin Polymers 0.000 claims description 21
- 239000011347 resin Substances 0.000 claims description 21
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 19
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 16
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 12
- 239000003729 cation exchange resin Substances 0.000 claims description 12
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 230000002209 hydrophobic effect Effects 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 claims description 4
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical compound CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 claims description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- QWOVEJBDMKHZQK-UHFFFAOYSA-N 1,3,5-tris(3-trimethoxysilylpropyl)-1,3,5-triazinane-2,4,6-trione Chemical compound CO[Si](OC)(OC)CCCN1C(=O)N(CCC[Si](OC)(OC)OC)C(=O)N(CCC[Si](OC)(OC)OC)C1=O QWOVEJBDMKHZQK-UHFFFAOYSA-N 0.000 claims description 3
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 3
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 claims description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 2
- YIKSHDNOAYSSPX-UHFFFAOYSA-N 1-propan-2-ylthioxanthen-9-one Chemical compound S1C2=CC=CC=C2C(=O)C2=C1C=CC=C2C(C)C YIKSHDNOAYSSPX-UHFFFAOYSA-N 0.000 claims description 2
- LWRBVKNFOYUCNP-UHFFFAOYSA-N 2-methyl-1-(4-methylsulfanylphenyl)-2-morpholin-4-ylpropan-1-one Chemical compound C1=CC(SC)=CC=C1C(=O)C(C)(C)N1CCOCC1 LWRBVKNFOYUCNP-UHFFFAOYSA-N 0.000 claims description 2
- KTALPKYXQZGAEG-UHFFFAOYSA-N 2-propan-2-ylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(C(C)C)=CC=C3SC2=C1 KTALPKYXQZGAEG-UHFFFAOYSA-N 0.000 claims description 2
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 claims description 2
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 2
- UGVRJVHOJNYEHR-UHFFFAOYSA-N 4-chlorobenzophenone Chemical compound C1=CC(Cl)=CC=C1C(=O)C1=CC=CC=C1 UGVRJVHOJNYEHR-UHFFFAOYSA-N 0.000 claims description 2
- FXIVKZGDYRLHKF-UHFFFAOYSA-N C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 Chemical compound C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 FXIVKZGDYRLHKF-UHFFFAOYSA-N 0.000 claims description 2
- 239000005046 Chlorosilane Substances 0.000 claims description 2
- NQSMEZJWJJVYOI-UHFFFAOYSA-N Methyl 2-benzoylbenzoate Chemical compound COC(=O)C1=CC=CC=C1C(=O)C1=CC=CC=C1 NQSMEZJWJJVYOI-UHFFFAOYSA-N 0.000 claims description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 2
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 2
- FZUGPQWGEGAKET-UHFFFAOYSA-N parbenate Chemical compound CCOC(=O)C1=CC=C(N(C)C)C=C1 FZUGPQWGEGAKET-UHFFFAOYSA-N 0.000 claims description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 2
- 239000002318 adhesion promoter Substances 0.000 claims 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 21
- 238000001723 curing Methods 0.000 description 21
- 238000009792 diffusion process Methods 0.000 description 21
- 238000003756 stirring Methods 0.000 description 15
- 239000003292 glue Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 239000007795 chemical reaction product Substances 0.000 description 8
- 238000002329 infrared spectrum Methods 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 4
- 229910002808 Si–O–Si Inorganic materials 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000003848 UV Light-Curing Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009194 climbing Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- URDOJQUSEUXVRP-UHFFFAOYSA-N 3-triethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C(C)=C URDOJQUSEUXVRP-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
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241001060310 Styracaceae Species 0.000 description 1
- 235000001361 Styrax officinalis Nutrition 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 235000019382 gum benzoic Nutrition 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides an organosilicon die-bonding adhesive and a preparation method and application thereof. The organic silicon die bonding adhesive comprises the following components in parts by mass: 100 parts of methyl propenyl silicone resin, 0.04-0.25 part of catalyst, 0.3-1 part of photoinitiator, 0.5-3 parts of tackifier and 5-35 parts of white carbon black; wherein the methacrylic silicone resin is a silicone resin containing hydroxyl groups, alkoxy groups and methacrylic groups. According to the invention, the methylpropenyl is introduced into the silicone resin, so that an ultraviolet-heating dual-curing system is realized, the organic silicon die-bonding adhesive is quickly cured and molded by ultraviolet curing, the pollution of a chip electrode can be avoided, and the ultraviolet-heating dual-curing system has higher thrust, particularly high-temperature thrust, than the traditional organic silicon die-bonding adhesive.
Description
Technical Field
The invention belongs to the technical field of semiconductor light-emitting chip packaging, and particularly relates to an organic silicon die bond adhesive and a preparation method and application thereof.
Background
LED Die bonding is also known as Die Bond or Die attach. Die bonding is a process in which a die is bonded to a designated area of a support by a glue (typically a conductive or insulating glue for LEDs) to form a thermal or electrical path that provides conditions for subsequent wire bonding.
The LED bracket is formed by injection molding PPA on the surface of an electric and heat conducting metal, plays a role in bearing an LED wafer and die bonding glue, is generally a copper silver-plated or gold-plated bracket, and has the effect of facilitating LED light emission and bonding with an LED gold wire, so that the LED chip and an LED bracket pin are conducted to form a loop, and the LED emits light.
However, due to the quality of electroplating of different manufacturers, the thickness, the uniformity and the integrity of metal plating layers of different brackets and the cleanliness of organic matters used in the electroplating process are different, so that the problem of whether the organic matters of the die bonding glue have diffusivity on the surface of the bracket is directly influenced.
Meanwhile, the current LED display screen is developed towards the directions of continuously reducing the dot spacing, rapidly increasing the pixel density and greatly improving the resolution, and along with the reduction of the dot spacing, the product packaging technology is more and more difficult, so that reasonable design and good manufacturing process are required to support, the product size is continuously reduced, the effective bonding pads capable of fixing the crystal are smaller, the interval between the bonding pads is smaller, the conventional functional area design is that the interval area is slightly concave, or the bonding pads are provided with a certain step from the interval area, and the bonding pad area is smaller, so that the required chip size is larger, the die bonding force is insufficient or bonding wires fail or cold bonding caused by the diffusion of the die bonding conductive glue are influenced, and the lamp is dead.
In the prior art, the organic silicon resin is adopted for bonding, and is widely applied to the LED packaging industry at present due to the low refractive index and excellent high and low temperature resistance, yellowing resistance, heat resistance and the like, but the organic silicon resin has lower polarity compared with other resin systems such as epoxy, acrylic acid and the like, so that the problem of diffusion on the surfaces of some LED brackets is more likely to occur, thereby causing cold joint and even welding failure.
In addition, wire bonding in the LED die attach process fails due in part to the volatilization of reactive small molecules of the die attach adhesive during high temperature curing, which is deposited on the pad of the chip.
Therefore, a die bond adhesive with high thrust, diffusion prevention and no chip pollution is needed, and the production yield of the LED package and the reliability of the product are improved.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an organic silicon die-bonding adhesive and a preparation method and application thereof.
In a first aspect, the invention provides an organic silicon die-bonding adhesive, which comprises the following components in parts by mass:
The methyl propenyl silicone resin is silicone resin containing hydroxyl, alkoxy and methyl propenyl.
As a specific embodiment of the invention, the methyl propenyl of the methyl propenyl silicone resin accounts for 5-50% of the mole ratio, and the degree of alkoxy hydrolysis is 20-70%; preferably, the molar ratio of the methylpropenyl groups is 5 to 20% and the degree of hydrolysis of the alkoxy groups is 41.6 to 60%.
According to the invention, the principle of UV curing can be utilized to ensure that the die-bonding glue reaches a certain degree of crosslinking in a quick time to form a polymer product with a certain network structure, so that on one hand, the capillary phenomenon caused by inconsistent quality of a bracket coating or diffusion caused by various reasons such as mismatching of the polarity of the surface of the coating with silica gel can be avoided; on the other hand, the diffusion phenomenon caused by the viscosity reduction of the die bond adhesive in the heating process can not occur.
As specific embodiments of the invention, the preparation raw materials of the methyl propenyl silicone resin comprise methyl trimethoxysilane, methacryloxypropyl trimethoxysilane, cation exchange resin and methanol.
According to the invention, the molecular structure of methyltrimethoxysilane which is a raw material for preparing the methacrylic silicon resin contains a silicon atom and three methoxy groups, and the groups can react with active groups such as hydroxyl groups in other raw materials to form a cross-linked structure. The methyltrimethoxysilane and the methacryloxypropyl trimethoxysilane both have three methoxy groups to form a T-shaped structure, so that the obtained methylpropenyl silicone resin has a specific T-shaped space network structure, the crosslinking degree of the obtained organosilicon crystal-fixing adhesive is increased, the resin strength is improved, and the thrust value is improved.
As a specific embodiment of the invention, the preparation method of the methyl propenyl silicone resin comprises the following steps:
S1: mixing methyltrimethoxysilane, methacryloxypropyl trimethoxysilane, a cation exchange resin and methanol to obtain a first mixture;
S2: adding water into the first mixture obtained in the step S1 according to the degree of hydrolysis, and mixing to obtain a second mixture;
S3: and refluxing, filtering and distilling the second mixture to obtain the methacrylic silicon resin.
As a specific embodiment of the invention, in the step S1, the mass ratio of the methyltrimethoxysilane, the methacryloxypropyl trimethoxysilane, the cation exchange resin and the methanol is 100 (9.6-45.6): 11.17-18.85): 14.84-25.03.
In the specific embodiment of the present invention, in the step S2, the water addition amount is added according to the degree of hydrolysis, preferably, the water addition amount is 14.0 to 22.2% by mass, and more preferably, 15.8 to 20.7% by mass of the total mass of methyltrimethoxysilane and methacryloxypropyl trimethoxysilane.
In the step S3, the reflux condition includes a temperature of 50-70 ℃ and a reflux time of 4-6 hours; the distillation comprises reduced pressure distillation under conditions including 100-130deg.C for 0.5-3 hr.
As specific embodiments of the present invention, the photoinitiator is diphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide, ethyl 2,4, 6-trimethylbenzoyl phenylphosphonate, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-methyl-1- (4-methylthiophenyl) -2-morpholino-1-propanone, 2-isopropylthioxanthone (2, 4 isomer mixture), ethyl 4-dimethylamino-benzoate, 1-hydroxy-cyclohexyl-phenyl methanone, 2-hydroxy-2-methyl-1-phenyl-1-propanone; at least one of dimethyl ether of the storax, methyl o-benzoyl benzoate, 4-chlorobenzophenone and isopropyl thioxanthone.
As a specific embodiment of the present invention, the tackifier is at least one of γ - (2, 3-glycidoxypropyl) trimethoxysilane, γ -methacryloxypropyl trimethoxysilane, γ - (2, 3-glycidoxypropyl) propyl triethoxysilane, γ -methacryloxypropyl triethoxysilane, γ -mercaptopropyl trimethoxysilane, γ -mercaptopropyl triethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (β -methoxyethoxy) silane, 3-mercaptopropyl methyldimethoxysilane, 1,3, 5-tris (trimethoxysilylpropyl) isocyanurate, triallyl isocyanurate.
As a specific embodiment of the present invention, the catalyst is diisopropyl di (acetylacetonate) titanate.
As a specific embodiment of the present invention, the white carbon black is hydrophobic white carbon black; preferably, the hydrophobic white carbon black includes a hydrophobic white carbon black treated with hexamethylsilazane or chlorosilane.
In a second aspect, the invention provides a preparation method of the organic silicon die-bonding adhesive in the first aspect, which is characterized in that the organic silicon die-bonding adhesive is obtained by uniformly mixing methyl propenyl silicone resin, a catalyst, a photoinitiator, a tackifier and white carbon black.
As a specific embodiment of the invention, the mixing condition comprises stirring and mixing, wherein the stirring speed is 200-500rmp, and the stirring time is 10-60min; the uniform mixing also comprises uniform dispersion, preferably, dispersing by a dispersing machine.
The above-mentioned raw materials in the present invention are all self-made or commercially available, and the present invention is not particularly limited thereto.
In a third aspect, the invention provides an application of the organic silicon die-bonding adhesive in the first aspect or the organic silicon die-bonding adhesive prepared by the preparation method in the second aspect in the field of LEDs.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the organic silicon die-bonding adhesive, the polarity of resin is improved by utilizing hydroxyl, and the methyl propenyl has the characteristic of combining ultraviolet rapid curing, so that on one hand, the polarity of resin is increased, and the diffusion risk of main resin of the organic silicon die-bonding adhesive on an LED bracket is reduced; on the other hand, by utilizing the principle of ultraviolet rapid curing, the die bond adhesive is rapidly and primarily cured, and the diffusion of the main resin of the die bond adhesive caused by capillary action can be effectively prevented. Meanwhile, the methyltrimethoxysilane in the die bonding adhesive has a three-dimensional network structure formed by ultraviolet curing, and can not be deposited on a chip electrode due to volatilization or adhesive climbing in the later high-temperature curing process, so that the occurrence of chip pollution is completely avoided. Particularly, the crystal-fixing glue prepared by adopting the methyltrimethoxysilane with a T-shaped structure has a specific T-shaped space network structure, the crosslinking degree is higher, the resin strength is improved, and the thrust value is improved.
2. The organic silicon die-bonding adhesive disclosed by the invention is simple in preparation method, environment-friendly in raw materials, cost-saving and suitable for wide popularization.
Drawings
FIG. 1 is an infrared spectrum of a methylpropenyl silicone resin obtained in example 1 of the present invention;
FIG. 2 is an infrared spectrum of a methylpropenyl silicone resin obtained in example 2 of the present invention;
FIG. 3 is an infrared spectrum of the silicone resin obtained in comparative example 1 of the present invention;
FIG. 4 is an infrared spectrum of the silicone resin obtained in comparative example 2 of the present invention;
FIG. 5 is a graph showing the diffusion of the cured die bond adhesive of example 3 according to the present invention;
FIG. 6 is a graph showing the diffusion of the cured die bond adhesive of example 4 under a microscope;
FIG. 7 is a graph showing the diffusion of the cured die bond adhesive of example 5 according to the present invention;
FIG. 8 is a graph showing the diffusion of the die bond adhesive of comparative example 3 after curing under a microscope;
FIG. 9 is a view showing the diffusion of a certain type of native die bond adhesive after curing under a microscope;
FIG. 10 is a graph of the diffusion of a commercial, imported die bond OE-8021 after curing, as observed under a microscope;
FIG. 11 is a graph showing the pollution test results of a die attach adhesive chip according to example 3 of the present invention;
FIG. 12 is a graph showing the results of the test for the contamination of the die bond adhesive chip of comparative example 3 of the present invention;
FIG. 13 is a graph showing the pollution test results of a die attach adhesive chip according to example 5 of the present invention;
FIG. 14 is a graph showing the pollution test results of a die attach adhesive chip according to example 4 of the present invention;
FIG. 15 is a graph showing the pollution test results of a chip of a certain type of domestic die bond;
FIG. 16 is a graph of the results of a commercially available OE-8021 chip contamination test.
Detailed Description
The invention is further illustrated below in connection with specific examples, which are not to be construed as limiting the invention in any way.
The information for each reagent used in the examples of the present invention is as follows:
The white carbon black is hydrophobic white carbon black obtained by dimethyl dichlorosilane treatment;
the catalyst is diisopropyl di (acetyl acetonyl) titanate;
a photoinitiator 1173d, 2-hydroxy-2-methyl-1-phenylpropiophenone;
cation exchange resin AMBERLYST 15WET;
Examples 1-2 are preparation examples of methacrylic silicone resins:
Example 1
The embodiment provides a methyl propenyl silicone resin and a preparation method thereof, and the specific details are as follows:
S1: 137.04g of methyltrimethoxysilane, 59.03g of methacryloxypropyl trimethoxysilane, 19.91g of cation exchange resin and 33.75g of methanol are sequentially added into a flask equipped with a condenser, a stirring rod and a thermometer, and the mixture is uniformly mixed at room temperature to obtain a first mixture;
S2: dropwise adding 28.29g of deionized water into the first mixture obtained in the step S1, stirring while dropwise adding, wherein the stirring speed is 200rmp, and reacting at 60 ℃ for 5 hours after the temperature is not increased any more to obtain a reaction product;
S3: and (3) cooling the reaction product obtained in the step (S2) to room temperature, filtering, distilling the filtrate under reduced pressure, and maintaining the temperature at 120 ℃ for 1h to obtain the methylpropenyl silicone resin.
The molar percentage of methylpropenyl in the methylpropenyl silicone resin obtained in example 1 was 20%, the degree of alkoxy hydrolysis was 41.6%, and the product viscosity was 165cs.
As shown in fig. 1, the infrared spectrum shows a characteristic absorption peak with a 3438cm -1 broad peak as-OH, 1028cm -1、845cm-1 as a characteristic absorption peak of Si-O-Si chain, 1720cm -1 and 1638cm -1 as characteristic absorption peaks of acryloyloxy group; a stretching vibration peak of 2841cm -1SiO-CH3.
Example 2
The embodiment provides a methyl propenyl silicone resin and a preparation method thereof, and the specific details are as follows:
s1: 163.46g of methyltrimethoxysilane, 31.24g of methacryloxypropyl trimethoxysilane, 19.91g of cation exchange resin and 35.72g of methanol are sequentially added into a flask provided with a condenser, a stirring rod and a thermometer, and the mixture is uniformly mixed at room temperature to obtain a first mixture;
s2: dropwise adding 43.19g of deionized water into the first mixture obtained in the step S1, stirring while dropwise adding, wherein the stirring speed is 200rmp, and reacting for 5 hours at 65 ℃ after the temperature is not increased any more to obtain a reaction product;
s3: and (3) cooling the reaction product obtained in the step (S2) to room temperature, filtering, distilling the filtrate under reduced pressure, and maintaining the temperature at 110 ℃ for 1h to obtain the methylpropenyl silicone resin.
The molar percentage of methylpropenyl in the methylpropenyl silicone resin obtained in example 2 was 10%, the degree of hydrolysis of alkoxy group was 60%, and the viscosity of the product was 20000cs.
As shown in FIG. 2, the infrared spectrum shows that 3393cm -1 wide peak is a characteristic absorption peak of-OH, 1008cm -1 is a characteristic absorption peak of Si-O-Si chain, 1720cm -1、1699cm-1 and 1638cm -1 are characteristic absorption peaks of acryloyloxy group; a stretching vibration peak of 2843cm -1SiO-CH3.
Comparative example 1
The comparative example provides a silicon-containing resin and a preparation method thereof, and the specific details are as follows:
s1: 216g of methyltrimethoxysilane, 25.7g of cation exchange resin and 36g of methanol are sequentially added into a flask provided with a condenser, a stirring rod and a thermometer, and the mixture is uniformly mixed at room temperature to obtain a first mixture;
S2: dropwise adding 51.37g of deionized water into the first mixture obtained in the step S1, stirring while dropwise adding, wherein the stirring speed is 200rmp, and reacting at 60 ℃ for 5 hours after the temperature is not increased any more to obtain a reaction product;
S3: and (3) cooling the reaction product obtained in the step (S2) to room temperature, filtering, distilling the filtrate under reduced pressure, and maintaining the temperature at 120 ℃ for 1h to obtain the silicon-containing resin.
The silicon-containing resin obtained in comparative example 1 had a molar percentage of methylpropenyl group of 0 and a degree of alkoxy hydrolysis of 60%. As shown in FIG. 3, the infrared spectrum showed 3418cm -1 as a characteristic absorption peak of-OH, and 1720cm -1 and 1638cm -1 as characteristic absorption peaks of no acryloyloxy group. 1021cm -1 is the characteristic absorption peak of the Si-O-Si chain, and 2843cm -1SiO-CH3 is the stretching vibration peak.
Comparative example 2
S1: 196.04g of methacryloxypropyl trimethoxysilane, 19.91g of cation exchange resin and 33.75g of methanol are added in sequence into a flask equipped with a condenser, a stirring rod and a thermometer, and the mixture is uniformly mixed at room temperature to obtain a first mixture;
s2: dropwise adding 18.79g of deionized water into the first mixture obtained in the step S1, stirring while dropwise adding, wherein the stirring speed is 200rmp, and reacting at 60 ℃ for 5 hours after the temperature is not increased any more to obtain a reaction product;
S3: and (3) cooling the reaction product obtained in the step (S2) to room temperature, filtering, distilling the filtrate under reduced pressure, and maintaining the temperature at 120 ℃ for 1h to obtain the methylpropenyl silicone resin.
The molar percentage of methylpropenyl in the methylpropenyl silicone resin obtained in comparative example 2 was 100%, and the degree of alkoxy hydrolysis was 41.6%.
As shown in fig. 4, the infrared spectrum shows that 3489cm -1 has a broad peak as a characteristic absorption peak of-OH, 1028cm -1 has a characteristic absorption peak of Si-O-Si chain, 1717cm -1 and 1638cm -1 have a characteristic absorption peak of acryloyloxy group; 2841cm -1 is the stretching vibration peak of SiO-CH 3.
Example 3
The embodiment provides an organic silicon die-bonding adhesive and a preparation method thereof, and the specific details are as follows:
50g of methylpropenyl silicone resin of example 1, 17.5g of white carbon black, 0.65g of gamma-glycidol ether oxypropyl trimethoxy silane, 0.035g of catalyst and 0.037g of photoinitiator 1173D are mixed and stirred uniformly, and then the mixture is placed in a rotation revolution dispersing machine for uniform dispersion, thus obtaining the organic silicon crystal-fixed glue.
Example 4
The embodiment provides an organic silicon die-bonding adhesive and a preparation method thereof, and the specific details are as follows:
25g of methyl propenyl silicone resin in example 1, 25g of methyl propenyl silicone resin in example 2, 10g of white carbon black, 0.65g of gamma-glycidol ether oxypropyl trimethoxy silane, 0.035g of catalyst and 0.037g of photoinitiator are mixed and stirred uniformly, and then the mixture is placed in a rotation revolution dispersing machine for uniform dispersion, thus obtaining the organic silicon crystal-fixed adhesive.
Example 5
50G of methylpropenyl silicone resin of example 2, 5g of white carbon black, 0.65g of gamma-glycidol ether oxypropyl trimethoxy silane, 0.035g of catalyst and 0.037g of photoinitiator 1173D are mixed and stirred uniformly, and the mixture is placed in a rotation revolution dispersing machine for uniform dispersion, thus obtaining the organic silicon crystal-fixed glue.
Example 6
25G of methyl propenyl silicone resin of example 1, 25g of methyl propenyl silicone resin of example 2, 10g of white carbon black, 0.5g of 1,3, 5-tris (trimethoxysilylpropyl) isocyanurate, 0.25g of gamma-mercaptopropyl trimethoxysilane, 0.035g of catalyst and 0.037g of photoinitiator are weighed according to the measurement, mixed and stirred uniformly, and placed in a rotation revolution dispersing machine for uniform dispersion, thus obtaining the organic silicon crystal-fixing adhesive.
Comparative example 3
The comparative example provides an organosilicon die-bonding adhesive and a preparation method thereof, and the specific details are as follows:
50g of silicon resin of comparative example 1, 10g of white carbon black, 0.65g of gamma-glycidol ether oxypropyl trimethoxy silane, 0.035g of diisopropyl di (acetyl) titanate catalyst and 0.037g of photoinitiator are mixed and stirred uniformly, and then the mixture is placed in a rotation revolution dispersing machine for uniform dispersion, thus obtaining the organosilicon crystal-fixing glue.
Comparative example 4
The comparative example provides an organosilicon die-bonding adhesive and a preparation method thereof, and the specific details are as follows:
25g of methylpropenyl silicone resin of comparative example 2, 17.5g of white carbon black, 0.035g of catalyst and 0.037g of photoinitiator 1173D are weighed according to the measurement, mixed and stirred uniformly, and placed in a rotation revolution dispersing machine to be dispersed uniformly, thus obtaining the organic silicon crystal-fixed glue.
Test case
The organosilicon die bond prepared in examples 3-4, comparative example 3 and comparative example 4 were tested in comparison with a type of domestic die bond, and with commercially available die bond OE-8021:
thrust testing
The LED luminous chips with the thickness of 8.13mil are adhered to PPA silver plating brackets which are common in the market by adopting the die bond adhesives, are pre-cured for 100S in an ultraviolet curing box, are then cured for 4 hours at 150 ℃, and are tested for thrust values at different temperatures including normal temperature, 160 ℃ and 250 ℃ by utilizing Dage 4000. The test results are shown in table 1:
TABLE 1 thrust testing of different die bond adhesives at different temperatures
Stent diffusion test
And dispensing each die bond adhesive onto a gold-plated bracket which is easy to diffuse, pre-curing for 100S in an ultraviolet curing box, curing for 4 hours at 150 ℃, and observing the diffusion condition under a microscope, wherein the diffusion result is shown in figures 5-10.
The chip contamination test is performed by a test method,
And (3) respectively coating the die bond adhesive with the thickness of 150 microns on the glass slide, placing a certain number of chips on the die bond adhesive, and then loading the thick glass sheet for sealing. Pre-curing for 100S in an ultraviolet curing box, and then placing in an oven at 150 ℃ for curing for 4 hours, and the pollution results are shown in fig. 11-15.
As can be seen from table 1 and fig. 1 to 9, the organic silicon die bond adhesives of examples 3 to 4 and the die bond adhesives of comparative examples 3 to 4 are both MT structures, and have high crosslinking density after curing, even though there is still high thrust on the LED light emitting chip of 8 x 13mil, at the same time, the thrust is still higher than the requirements of the commercial products and industries at the high temperature of 160 ℃ and 250 ℃, and the die bond adhesive is not at risk of die drop in the whole LED package preparation process.
The methylpropenyl silicone resins of the embodiment 3 and the embodiment 4 are respectively introduced with the methylpropenyl, so that the prepared organic silicon crystal-fixing glue can achieve a certain degree of crosslinking in a rapid time by utilizing the principle of UV curing, and a polymer product with a certain network structure is formed, so that on one hand, the diffusion caused by capillary phenomenon caused by inconsistent quality of a bracket coating or multiple reasons such as mismatching of the polarity of the surface of the coating with silica gel is avoided; on the other hand, the diffusion caused by the viscosity reduction of the die bond adhesive in the heating process can not be caused.
The die bond adhesive in comparative example 3 does not introduce a functional group methylpropenyl capable of being cured by UV, and obviously has a certain diffusion phenomenon on the surface of the LED bracket. In contrast, in comparative example 4, too much cross-linking degree of the product caused by too much introduction of the methacrylic group resulted in high temperature cracking, resulting in extremely low thrust.
From the chip electrode pollution test, the die bond adhesive of comparative example 3 and a certain domestic die bond adhesive have more or less chip pollution, and the embodiment 3 does not show chip pollution because the introduction of the front-stage methylpropenyl of the die bond adhesive obtained in the embodiment 3 leads the die bond adhesive to initially form a three-dimensional network structure before high-temperature curing, thereby effectively avoiding bonding wire failure caused by volatile deposition of reactive micromolecules on a chip pad.
In summary, the organic silicon die-bonding adhesive disclosed by the invention has the advantages that the polarity of the resin is improved by utilizing hydroxyl, and the methyl propenyl has the characteristic of combining ultraviolet rapid curing, so that on one hand, the polarity of the resin is increased, and the diffusion risk of the main resin of the organic silicon die-bonding adhesive on an LED bracket is reduced; on the other hand, by utilizing the principle of ultraviolet rapid curing, the die bond adhesive is rapidly and primarily cured, and the diffusion of the main resin of the die bond adhesive caused by capillary action can be effectively prevented. Meanwhile, the methyltrimethoxysilane in the die bonding adhesive has a three-dimensional network structure formed by ultraviolet curing, and can not be deposited on a chip electrode due to volatilization or adhesive climbing in the later high-temperature curing process, so that the occurrence of chip pollution is completely avoided. Particularly, the crystal-fixing glue prepared by adopting the methyltrimethoxysilane with a T-shaped structure has a specific T-shaped space network structure, the crosslinking degree is higher, the resin strength is improved, and the thrust value is improved.
Any numerical value recited in this disclosure includes all values incremented by one unit from the lowest value to the highest value if there is only a two unit interval between any lowest value and any highest value. For example, if the amount of a component, or a process variable such as temperature, pressure, time, etc., is stated to be 50-90, it is meant in this specification that values such as 51-89, 52-88 … …, and 69-71, and 70-71 are specifically recited. For non-integer values, 0.1, 0.01, 0.001 or 0.0001 units may be considered as appropriate. This is only a few examples of the specific designations. In a similar manner, all possible combinations of values between the lowest value and the highest value enumerated are to be considered to be disclosed.
It should be noted that the above-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.
Claims (13)
1. The organic silicon die bonding adhesive is characterized by comprising the following components in parts by mass:
100 parts of methyl propenyl silicone resin,
0.04-0.25 Parts of catalyst,
0.3-1 Part of photoinitiator,
0.5-3 Parts of tackifier,
5-35 Parts of white carbon black;
the methyl propenyl silicone resin is silicone resin containing hydroxyl, alkoxy and methyl propenyl,
Wherein, the preparation raw materials of the methyl propenyl silicone resin comprise methyl trimethoxy silane, methacryloxypropyl trimethoxy silane, cation exchange resin and methanol;
Wherein the mass ratio of the methyltrimethoxysilane to the methacryloxypropyl trimethoxysilane to the cation exchange resin to the methanol is 100 (9.0-43.0): (11.17-18.85): (14.84-25.03).
2. The die bond adhesive of claim 1, wherein the methyl propenyl silicone resin has a methyl propenyl molar ratio of 5% -50% and an alkoxy hydrolysis degree of 20% -70%.
3. The die bond adhesive according to claim 2, wherein the methyl propenyl silicone resin has a methyl propenyl molar ratio of 5-20% and an alkoxy hydrolysis degree of 41.6-60%.
4. A die attach adhesive as claimed in any one of claims 1 to 3, wherein the method of preparing the methylpropenyl silicone resin comprises the steps of:
S1: mixing methyltrimethoxysilane, methacryloxypropyl trimethoxysilane, a cation exchange resin and methanol to obtain a first mixture;
S2: adding water into the first mixture obtained in the step S1 according to the degree of hydrolysis, and mixing to obtain a second mixture;
S3: and refluxing, filtering and distilling the second mixture to obtain the methacrylic silicon resin.
5. The die bond adhesive according to claim 4, wherein in the step S1, the mass ratio of methyltrimethoxysilane, methacryloxypropyl trimethoxysilane, cation exchange resin and methanol is 100 (9.0-43.0): (11.17-18.85): (14.84-25.03); and
In the step S2, the water adding amount is added according to the degree of hydrolysis; and/or
In the step S3, the reflux condition comprises that the temperature is 50-70 ℃ and the reflux time is 4-6h; the distillation comprises reduced pressure distillation under conditions including 100-130deg.C for 0.5-3 hr.
6. The die bond adhesive according to claim 5, wherein in the step S2, the water addition amount is 14.0-22.2% of the total mass of methyltrimethoxysilane and methacryloxypropyl trimethoxysilane.
7. The die bond adhesive of claim 6, wherein in the step S2, the water addition amount is 15.8-20.7% of the total mass of methyltrimethoxysilane and methacryloxypropyl trimethoxysilane.
8. A die bond adhesive according to any one of claims 1-3, wherein the photoinitiator is at least one of diphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide, ethyl 2,4, 6-trimethylbenzoyl phenylphosphonate, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-methyl-1- (4-methylthiophenyl) -2-morpholino-1-propanone, 2-isopropylthioxanthone (2, 4 isomer mixture), ethyl 4-dimethylamino-benzoate, 1-hydroxy-cyclohexyl-phenyl methanone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, cyroman dimethyl ether, methyl o-benzoyl benzoate, 4-chlorobenzophenone, isopropyl thioxanthone.
9. A die bond adhesive according to any one of claims 1 to 3, wherein the adhesion promoter is at least one of gamma- (2, 3-glycidoxypropyl) trimethoxysilane, gamma-methacryloxypropyl trimethoxysilane, gamma- (2, 3-glycidoxypropyl) triethoxysilane, gamma-methacryloxypropyl triethoxysilane, gamma-mercaptopropyl trimethoxysilane, gamma-mercaptopropyl triethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (β -methoxyethoxy) silane, 3-mercaptopropyl methyldimethoxy silane, 1,3, 5-tris (trimethoxysilylpropyl) isocyanurate, triallyl isocyanurate;
and/or the catalyst is diisopropyl di (acetylacetonate) titanate.
10. A die attach adhesive as claimed in any one of claims 1 to 3 wherein the white carbon black is hydrophobic white carbon black.
11. The die attach adhesive of claim 10 wherein the hydrophobic white carbon comprises a hydrophobic white carbon treated with hexamethylsilazane or chlorosilane.
12. The method for preparing the organic silicon die-bonding adhesive according to any one of claims 1 to 11, which is characterized in that the organic silicon die-bonding adhesive is obtained by uniformly mixing methyl propenyl silicone resin, a catalyst, a photoinitiator, a tackifier and white carbon black.
13. Use of the silicone die attach adhesive of any one of claims 1-11 or the silicone die attach adhesive prepared by the preparation method of claim 12 in the field of LEDs.
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