CN115851194A - Underfill with anti-overflow grease performance and preparation method thereof - Google Patents
Underfill with anti-overflow grease performance and preparation method thereof Download PDFInfo
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- 239000004519 grease Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 29
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 14
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 13
- 239000007822 coupling agent Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 claims abstract description 9
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 64
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 50
- 239000000203 mixture Substances 0.000 claims description 36
- 239000000377 silicon dioxide Substances 0.000 claims description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 16
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 claims description 10
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 10
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 10
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 10
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 9
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 9
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims description 8
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 7
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 7
- JJYPMNFTHPTTDI-UHFFFAOYSA-N 3-methylaniline Chemical compound CC1=CC=CC(N)=C1 JJYPMNFTHPTTDI-UHFFFAOYSA-N 0.000 claims description 6
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 claims description 5
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 claims description 5
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 5
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 4
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 3
- ZXUJYIQZKNWLQN-UHFFFAOYSA-N [3-(7-oxabicyclo[4.1.0]heptan-3-ylmethyl)-7-oxabicyclo[4.1.0]heptan-3-yl] formate Chemical compound C(=O)OC1(CC2C(CC1)O2)CC1CC2C(CC1)O2 ZXUJYIQZKNWLQN-UHFFFAOYSA-N 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- 239000003292 glue Substances 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 239000004721 Polyphenylene oxide Substances 0.000 description 7
- 150000001412 amines Chemical class 0.000 description 7
- 229920000570 polyether Polymers 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 229960001124 trientine Drugs 0.000 description 6
- -1 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formic ether Chemical compound 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the technical field of adhesives, and provides an underfill with anti-overflow performance and a preparation method thereof. The underfill comprises the following components in parts by weight: 20 to 40 parts of epoxy resin, 1 to 5 parts of coupling agent, 0.1 to 2 parts of dispersing agent, 10 to 25 parts of curing agent, 0.1 to 1 part of accelerator, 50 to 80 parts of filler and 1 to 10 parts of additive, wherein the additive is one or more of triglycidyl isocyanurate, aminophenol trifunctional epoxy resin and epoxidized m-benzhydrylamine. In the invention, the additive can enable the inside of the underfill to form a three-dimensional cross-linked network, and under the condition that the adhesive force of the underfill to the substrate is not changed, higher cohesive force is obtained so as to inhibit the phenomenon of grease overflow; the compounding of other components can make the filling glue have lower thermal expansion coefficient and better fluidity, and can ensure the reliability of chip packaging.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an underfill with anti-overflow performance and a preparation method thereof.
Background
The underfill is an epoxy resin encapsulating material, has high fluidity, high purity and single component, and can fill the gap at the bottom of the wafer (die) after heating and curing, thereby reinforcing the chip, strengthening the anti-drop performance and the reliability of the system, and reducing the stress impact between the wafer (die) and the substrate. The working principle is as follows: it utilizes capillary action to allow glue to flow rapidly across the bottom of the wafer (die) with a minimum flowable space of 10um, which also meets the electrical safety characteristics of the soldering process because glue does not flow in gaps below 4 um.
Epoxy-based underfills are commonly used, with silica fillers and various adjuvants added to achieve optimum performance. However, in practical packaging applications, a precipitation phenomenon is likely to occur on the surface of a chip, which becomes "fat overflow", and in the whole chip package, other package elements are also bonded on the surface of the chip, so that the fat overflow phenomenon affects subsequent packaging, and if serious, other components are polluted, so that the packaging reliability is reduced, and the product is unqualified. The reason for the flashing phenomenon is that some components of the underfill adhere to the substrate more than the cohesion of all of its components.
Therefore, how to provide an underfill having excellent anti-blooming properties is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the present invention provides an underfill with anti-bleeding property and a preparation method thereof. The technical problem that the grease overflowing phenomenon easily occurs in the existing underfill is solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an underfill with anti-overflow performance, which comprises the following components in parts by weight:
20 to 40 parts of epoxy resin, 1 to 5 parts of coupling agent, 0.1 to 2 parts of dispersant, 10 to 25 parts of curing agent, 0.1 to 1 part of accelerator, 50 to 80 parts of filler and 1 to 10 parts of additive;
the additive is one or more of triglycidyl isocyanurate, aminophenol trifunctional epoxy resin and epoxidized m-toluidine.
Furthermore, the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, p-aminophenol epoxy resin and 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formic ether.
Further, the coupling agent is one or more of 3- (2, 3-glycidoxy) propyl trimethoxy silane, (3-glycidoxypropyl) triethoxy silane, gamma-glycidoxypropyl trimethoxy silane and 3-aminopropyl methyl dimethoxy silane.
Further, the dispersant is one or more of TEGO900, BYK-110, BYK-323, BYK-333 and DISPERBYK-111.
Further, the curing agent is one or more of diethylenetriamine, triethylene tetramine, m-phenylenediamine, diethyl toluenediamine and polyether amine.
Further, the accelerant is one or more of triphenylphosphine, tetrabutyl titanate and isooctanoic acid.
Further, the filler is spherical silica; the spherical silicon dioxide is selected from one or more of spherical silicon dioxide with the particle size of 0.1-1 mu m, 3-8 mu m and 10-20 mu m.
The invention provides a preparation method of the underfill with the anti-overflow grease performance, which comprises the following steps:
s1, mixing epoxy resin, a coupling agent, a dispersing agent, a curing agent and an accelerating agent to obtain a mixture A;
s2, mixing the mixture A and the filler to obtain a mixture B;
and S3, mixing the mixture B with an additive, and performing vacuum defoaming after the mixing treatment to obtain the underfill with the anti-overflow performance.
Further, the temperature of the mixing treatment in the step S1 and the step S2 is 20-30 ℃ independently, and the time of the mixing treatment is 1-3 h independently.
Further, the temperature of the material mixing treatment in the step S3 is 60-100 ℃, and the time of the material mixing treatment is 4-8 hours;
and the vacuum defoaming time in the step S3 is 10-30 min.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
in the invention, the epoxy resin, the curing agent and the accelerator ensure the basic characteristics of the underfill, such as viscosity, reactivity, bonding strength, heat resistance and the like; the coupling agent improves the process characteristics of the underfill; the addition of the filler improves the characteristics of the underfill, such as the thermal expansion coefficient, the modulus and the like; the additive can enable the inside of the underfill to form a three-dimensional cross-linked network, and under the condition that the adhesive force of the underfill to the substrate is not changed, higher cohesive force is obtained, so that the grease overflow phenomenon is inhibited.
Detailed Description
The invention provides an underfill with anti-overflow performance, which comprises the following components in parts by weight:
20 to 40 portions of epoxy resin, 1 to 5 portions of coupling agent, 0.1 to 2 portions of dispersant, 10 to 25 portions of curing agent, 0.1 to 1 portion of accelerant, 50 to 80 portions of filler and 1 to 10 portions of additive.
In the present invention, the amount of the epoxy resin is preferably 22 to 36 parts, and more preferably 25 to 32 parts;
in the present invention, the amount of the coupling agent is preferably 2 to 4 parts, and more preferably 3 parts;
in the present invention, the amount of the dispersant is preferably 0.4 to 1.6 parts, and more preferably 0.8 to 1.2 parts;
in the present invention, the amount of the curing agent is preferably 13 to 22 parts, and more preferably 15 to 20 parts;
in the present invention, the amount of the accelerator is preferably 0.2 to 0.8 part, and more preferably 0.4 to 0.6 part;
in the present invention, the amount of the filler is preferably 55 to 75 parts, and more preferably 60 to 70 parts;
in the present invention, the amount of the additive is preferably 2 to 8 parts, and more preferably 4 to 7 parts.
In the invention, the additive is one or more of triglycidyl isocyanurate, aminophenol trifunctional epoxy resin and epoxidized m-toluidine, preferably triglycidyl isocyanurate and/or aminophenol trifunctional epoxy resin, and further preferably triglycidyl isocyanurate.
In the invention, the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, p-aminophenol epoxy resin and 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate, preferably one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, p-aminophenol epoxy resin and 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate, and further preferably bisphenol A epoxy resin and/or bisphenol F epoxy resin.
In the invention, the coupling agent is one or more of 3- (2, 3-glycidoxypropyl) propyltrimethoxysilane, (3-glycidoxypropyl) triethoxysilane, gamma-glycidoxypropyltrimethoxysilane and 3-aminopropylmethyldimethoxysilane, preferably one or more of 3- (2, 3-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and 3-aminopropylmethyldimethoxysilane, and more preferably gamma-glycidoxypropyltrimethoxysilane.
In the invention, the dispersant is one or more of TEGO900, BYK-110, BYK-323, BYK-333 and DISPERBYK-111, preferably one or more of TEGO900, BYK-110, BYK-323 and DISPERBYK-111, and further preferably one or more of TEGO900, BYK-323 and DISPERBYK-111.
In the invention, the curing agent is one or more of diethylenetriamine, triethylene tetramine, m-phenylenediamine, diethyl toluene diamine and polyether amine, preferably one or more of diethylenetriamine, triethylene tetramine, m-phenylenediamine and polyether amine, and further preferably one or more of triethylene tetramine, m-phenylenediamine and polyether amine.
In the invention, the promoter is one or more of triphenylphosphine, n-butyl titanate and isooctanoic acid, preferably n-butyl titanate and/or isooctanoic acid, and more preferably n-butyl titanate.
In the present invention, the filler is spherical silica; the spherical silicon dioxide is selected from one or more of spherical silicon dioxide with the particle size of 0.1-1 mu m, 3-8 mu m and 10-20 mu m, preferably the spherical silicon dioxide with the particle size of 3-8 mu m and/or 10-20 mu m, and more preferably the spherical silicon dioxide with the particle size of 3-8 mu m.
The invention provides a preparation method of the underfill with the anti-overflow grease performance, which comprises the following steps:
s1, mixing epoxy resin, a coupling agent, a dispersing agent, a curing agent and an accelerating agent to obtain a mixture A;
s2, mixing the mixture A and the filler to obtain a mixture B;
and S3, mixing the mixture B with an additive, and performing vacuum defoaming after the mixing treatment to obtain the underfill with the anti-overflow performance.
In the invention, the temperature of the mixing treatment in the step S1 and the step S2 is independently 20-30 ℃, preferably 22-26 ℃, and more preferably 25 ℃; the time for mixing treatment is independently 1-3 h, preferably 2h.
In the invention, the temperature of the mixing treatment in the step S3 is 60-100 ℃, preferably 65-90 ℃, and more preferably 70-80 ℃; the time for mixing treatment is 4-8 h, preferably 5-7 h, and further preferably 6h;
the time for vacuum defoaming in step S3 is 10 to 30min, preferably 15 to 25min, and more preferably 20min.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
Mixing 15 parts of bisphenol A epoxy resin, 15 parts of bisphenol F epoxy resin, 4 parts of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 1 part of BYK-323, 10 parts of m-phenylenediamine, 5 parts of polyether amine and 0.5 part of n-butyl titanate, and mixing at 25 ℃ for 2 hours to obtain a mixture A;
mixing the mixture A with 40 parts of spherical silicon dioxide with the particle size of 3-8 microns and 30 parts of spherical silicon dioxide with the particle size of 10-20 microns, and mixing the materials at 25 ℃ for 2 hours to obtain a mixture B;
and mixing the mixture B with 5 parts of triglycidyl isocyanurate, mixing for 6 hours at 80 ℃, and defoaming in vacuum for 20 minutes after the mixing treatment is finished to obtain the underfill with the anti-overflow grease performance.
Example 2
Mixing 20 parts of bisphenol A epoxy resin, 14 parts of bisphenol S epoxy resin, 3 parts of gamma-glycidoxypropyltrimethoxysilane, 1 part of TEGO900,1 part of BYK-323, 3 parts of triethylene tetramine, 5 parts of m-phenylenediamine, 5 parts of polyether amine and 0.8 part of isooctanoic acid, and mixing for 2 hours at 27 ℃ to obtain a mixture A;
mixing the mixture A with 20 parts of spherical silicon dioxide with the grain diameter of 3-8 mu m and 40 parts of spherical silicon dioxide with the grain diameter of 10-20 mu m, and mixing the materials at 27 ℃ for 2 hours to obtain a mixture B;
and mixing the mixture B with 5 parts of aminophenol trifunctional epoxy resin, mixing for 7 hours at the temperature of 80 ℃, and defoaming in vacuum for 30 minutes after the mixing treatment is finished to obtain the underfill with the anti-overflow grease performance.
Example 3
Mixing 10 parts of p-aminophenol epoxy resin, 15 parts of bisphenol F epoxy resin, 2 parts of (3-glycidoxypropyl) triethoxysilane, 1.5 parts of DISPERBYK-111, 5 parts of m-phenylenediamine, 8 parts of diethyl toluenediamine and 0.8 part of triphenylphosphine, and mixing at 26 ℃ for 3 hours to obtain a mixture A;
mixing the mixture A with 40 parts of spherical silicon dioxide with the particle size of 0.1-1 mu m and 40 parts of spherical silicon dioxide with the particle size of 10-20 mu m, and mixing the materials at 26 ℃ for 3 hours to obtain a mixture B;
and mixing the mixture B with 8 parts of epoxidized m-benzhydrylamine, mixing for 5 hours at 90 ℃, and defoaming for 30 minutes in vacuum after the mixing treatment is finished to obtain the underfill with the anti-overflow grease performance.
Example 4
Mixing 17 parts of bisphenol A epoxy resin, 10 parts of 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexyl formate, 2 parts of 3-aminopropylmethyldimethoxysilane, 1 part of BYK-110, 22 parts of diethyltoluenediamine and 0.5 part of n-butyl titanate, and mixing for 3 hours at 20 ℃ to obtain a mixture A;
mixing the mixture A with 30 parts of spherical silicon dioxide with the particle size of 3-8 microns and 30 parts of spherical silicon dioxide with the particle size of 0.1-1 micron, and mixing the materials at 20 ℃ for 3 hours to obtain a mixture B;
and mixing the mixture B with 3 parts of triglycidyl isocyanurate and 3 parts of epoxidized m-benzhydrylamine, mixing at 80 ℃ for 7 hours, and defoaming in vacuum for 30 minutes after the mixing treatment is finished to obtain the underfill with the anti-overflow grease performance.
Example 5
Mixing 35 parts of bisphenol A epoxy resin, 5 parts of gamma-glycidoxypropyltrimethoxysilane, 1 part of BYK-333, 18 parts of triethylene tetramine and 1.2 parts of triphenylphosphine, and mixing at 22 ℃ for 3 hours to obtain a mixture A;
mixing the mixture A, 20 parts of spherical silicon dioxide with the particle size of 10-20 microns, 20 parts of spherical silicon dioxide with the particle size of 3-8 microns and 20 parts of spherical silicon dioxide with the particle size of 0.1-1 microns, and mixing the materials at 22 ℃ for 3 hours to obtain a mixture B;
and mixing the mixture B with 2 parts of triglycidyl isocyanurate, 2 parts of epoxidized m-benzhydrylamine and 2 parts of aminophenol trifunctional epoxy resin, mixing for 6 hours at 100 ℃, and defoaming in vacuum for 30 minutes after the mixing treatment is finished to obtain the underfill with the anti-overflow performance.
Comparative example 1
Mixing 15 parts of bisphenol A epoxy resin, 15 parts of bisphenol F epoxy resin, 4 parts of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, 1 part of BYK-323, 10 parts of m-phenylenediamine, 5 parts of polyether amine and 0.5 part of n-butyl titanate, and mixing for 2 hours at 25 ℃ to obtain a mixture A;
mixing the mixture A with 40 parts of spherical silicon dioxide with the particle size of 3-8 microns and 30 parts of spherical silicon dioxide with the particle size of 10-20 microns, and mixing the materials at 25 ℃ for 2 hours to obtain a mixture B;
and (5) defoaming the mixture B in vacuum for 20min to obtain the underfill.
Performance testing
Viscosity test method: examples 1-5 and comparative examples were all tested using a parallel plate rheometer at 25 ℃ with a shear rate of 50s -1 The diameter of the rotor is 25mm, the clearance is 0.1mm, and the test results are shown in Table 1.
The thermal expansion coefficient test method comprises the following steps: the underfill prepared in examples 1 to 5 and comparative example was cured into a 2 × 5 × 5mm cube, the curing steps were as follows: firstly baking for 1h at 150 ℃, cooling to 100 ℃, baking for 2h, then heating to 150 ℃, baking for 1h to finish curing, and then testing by using a thermal mechanical analyzer, wherein the testing temperature interval is 30-250 ℃, the heating rate of the thermal mechanical analyzer during testing is 5 ℃/min, the tested thermal expansion coefficient is less than or equal to Tg, and the testing result is shown in table 1.
TABLE 1 determination of viscosity and thermal expansion coefficient of underfill
The method for measuring the length of the surface spilled grease comprises the following steps: observing and measuring the prepared simulation sample before and after curing under a high power microscope, respectively taking five position points on the other three edges except the dispensing edge on the bare silicon wafer, and measuring the distance from the outermost edge of the bare silicon wafer to the outermost edge of the grease overflow, namely the lengths of the grease overflow before and after curing are L respectively 0 And L, the results are shown in Table 2.
TABLE 2 test results for surface bleed length
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | |
| L 0 (μm) | 103 | 106 | 122 | 105 | 117 | 210 |
| L(μm) | 134 | 133 | 165 | 126 | 143 | 432 |
| Rate of change (%) | 30.1 | 25.5 | 26.7 | 20.0 | 22.2 | 105.7 |
As can be seen from the above tables 1 and 2, the underfill prepared by the present invention not only has the advantages of good viscosity, low thermal expansion coefficient, etc., but also has excellent anti-flash capability, and enhances the reliability of the package.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The underfill with the anti-overflow grease performance is characterized by comprising the following components in parts by weight:
20 to 40 parts of epoxy resin, 1 to 5 parts of coupling agent, 0.1 to 2 parts of dispersant, 10 to 25 parts of curing agent, 0.1 to 1 part of accelerator, 50 to 80 parts of filler and 1 to 10 parts of additive;
the additive is one or more of triglycidyl isocyanurate, aminophenol trifunctional epoxy resin and epoxidized m-toluidine.
2. The underfill of claim 1, wherein said epoxy resin is one or more of bisphenol a epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, p-aminophenol epoxy resin, and 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexyl formate.
3. The underfill according to claim 2, wherein the coupling agent is one or more of 3- (2, 3-glycidoxy) propyltrimethoxysilane, (3-glycidoxypropyl) triethoxysilane, gamma-glycidoxypropyltrimethoxysilane and 3-aminopropylmethyldimethoxysilane.
4. The underfill of any one of claims 1 to 3, wherein the dispersant is one or more of TEGO900, BYK-110, BYK-323, BYK-333 and DISPERBYK-111.
5. The underfill according to claim 4, wherein the curing agent is one or more selected from diethylenetriamine, triethylenetetramine, m-phenylenediamine, diethyltoluenediamine and polyetheramine.
6. The underfill according to claim 2,3 or 5 wherein the accelerator is one or more of triphenylphosphine, n-butyl titanate and isooctanoic acid.
7. The underfill according to claim 1 or 5, wherein the filler is spherical silica; the spherical silicon dioxide is selected from one or more of spherical silicon dioxide with the particle size of 0.1-1 mu m, 3-8 mu m and 10-20 mu m.
8. A process for the preparation of an underfill having anti-bleeding properties according to any one of claims 1 to 7, comprising the steps of:
s1, mixing epoxy resin, a coupling agent, a dispersing agent, a curing agent and an accelerating agent to obtain a mixture A;
s2, mixing the mixture A and the filler to obtain a mixture B;
and S3, mixing the mixture B with an additive, and performing vacuum defoaming after the mixing treatment to obtain the underfill with the anti-overflow performance.
9. The preparation method according to claim 8, wherein the temperature of the mixing treatment in the step S1 and the temperature of the mixing treatment in the step S2 are independently 20 to 30 ℃, and the time of the mixing treatment is independently 1 to 3 hours.
10. The preparation method according to claim 8 or 9, characterized in that the temperature of the mixing treatment in the step S3 is 60-100 ℃, and the time of the mixing treatment is 4-8 h;
and the vacuum defoaming time in the step S3 is 10-30 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211565473.7A CN115851194A (en) | 2022-12-07 | 2022-12-07 | Underfill with anti-overflow grease performance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202211565473.7A CN115851194A (en) | 2022-12-07 | 2022-12-07 | Underfill with anti-overflow grease performance and preparation method thereof |
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| CN115851194A true CN115851194A (en) | 2023-03-28 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439254A (en) * | 2018-10-31 | 2019-03-08 | 深圳广恒威科技有限公司 | A kind of reworkable high reliability filling glue |
| CN115160963A (en) * | 2022-08-08 | 2022-10-11 | 苏州宇川聚禾新材料有限公司 | High-temperature-resistant low-thermal-expansion-coefficient filling adhesive and preparation method thereof |
| CN115322718A (en) * | 2022-08-22 | 2022-11-11 | 深圳先进电子材料国际创新研究院 | Underfill adhesive and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439254A (en) * | 2018-10-31 | 2019-03-08 | 深圳广恒威科技有限公司 | A kind of reworkable high reliability filling glue |
| CN115160963A (en) * | 2022-08-08 | 2022-10-11 | 苏州宇川聚禾新材料有限公司 | High-temperature-resistant low-thermal-expansion-coefficient filling adhesive and preparation method thereof |
| CN115322718A (en) * | 2022-08-22 | 2022-11-11 | 深圳先进电子材料国际创新研究院 | Underfill adhesive and preparation method thereof |
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