CN117304855B - Epoxy adhesive for reinforcing BGA welding column and preparation method thereof - Google Patents
Epoxy adhesive for reinforcing BGA welding column and preparation method thereof Download PDFInfo
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- CN117304855B CN117304855B CN202311431449.9A CN202311431449A CN117304855B CN 117304855 B CN117304855 B CN 117304855B CN 202311431449 A CN202311431449 A CN 202311431449A CN 117304855 B CN117304855 B CN 117304855B
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- 230000003014 reinforcing effect Effects 0.000 title claims abstract description 80
- 229920006332 epoxy adhesive Polymers 0.000 title claims abstract description 69
- 238000003466 welding Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 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 48
- 229920001971 elastomer Polymers 0.000 claims abstract description 41
- 229920001021 polysulfide Polymers 0.000 claims abstract description 37
- 239000005077 polysulfide Substances 0.000 claims abstract description 37
- 150000008117 polysulfides Polymers 0.000 claims abstract description 37
- 239000003822 epoxy resin Substances 0.000 claims abstract description 33
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 33
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000003085 diluting agent Substances 0.000 claims abstract description 17
- 239000000945 filler Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 229910000679 solder Inorganic materials 0.000 claims description 46
- 229920006335 epoxy glue Polymers 0.000 claims description 26
- 239000004593 Epoxy Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 claims description 3
- UUODQIKUTGWMPT-UHFFFAOYSA-N 2-fluoro-5-(trifluoromethyl)pyridine Chemical compound FC1=CC=C(C(F)(F)F)C=N1 UUODQIKUTGWMPT-UHFFFAOYSA-N 0.000 claims description 3
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010456 wollastonite Substances 0.000 claims description 3
- 229910052882 wollastonite Inorganic materials 0.000 claims description 3
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- IPBVNPXQWQGGJP-UHFFFAOYSA-N acetic acid phenyl ester Natural products CC(=O)OC1=CC=CC=C1 IPBVNPXQWQGGJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000010425 asbestos Substances 0.000 claims description 2
- 239000000378 calcium silicate Substances 0.000 claims description 2
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 2
- 229930003836 cresol Natural products 0.000 claims description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 2
- 229940049953 phenylacetate Drugs 0.000 claims description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 claims description 2
- ARJOQCYCJMAIFR-UHFFFAOYSA-N prop-2-enoyl prop-2-enoate Chemical compound C=CC(=O)OC(=O)C=C ARJOQCYCJMAIFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052895 riebeckite Inorganic materials 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 7
- 239000012776 electronic material Substances 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 20
- 238000012360 testing method Methods 0.000 description 15
- 239000000853 adhesive Substances 0.000 description 12
- 230000001070 adhesive effect Effects 0.000 description 12
- 230000000694 effects Effects 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- RVCKCEDKBVEEHL-UHFFFAOYSA-N 2,3,4,5,6-pentachlorobenzyl alcohol Chemical compound OCC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl RVCKCEDKBVEEHL-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002508 compound effect Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Classifications
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- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The application relates to the technical field of electronic material preparation, and particularly discloses epoxy adhesive for reinforcing BGA (ball grid array) welding columns and a preparation method thereof. The epoxy adhesive for reinforcing the BGA welding column comprises an A component and a B component, wherein the A component comprises the following raw materials in parts by weight: 70-80 parts of bisphenol A type epoxy resin; 5-10 parts of carboxyl-terminated liquid nitrile rubber; 2-5 parts of polysulfide rubber; 3-7 parts of nano alumina whisker; 1-5 parts of a silane coupling agent; 10-15 parts of reactive diluent; 3-5 parts of filler; the component B consists of the following raw materials in parts by weight: 70-90 parts of curing agent; 2-6 parts of a promoter; the weight ratio of the component A to the component B is (2.2-3.8) 1; the preparation method comprises the following steps: mixing the raw materials of the component A to obtain a component A mixture; mixing the raw materials of the component B to obtain a component B mixture; and finally, uniformly mixing the component A mixture and the component B mixture to obtain the composite material. The epoxy adhesive for reinforcing the BGA welding column has excellent crack resistance in a cold-hot change environment, and can improve the reliability and service life of the BGA welding column.
Description
Technical Field
The application relates to the technical field of electronic material preparation, in particular to epoxy adhesive for reinforcing BGA (ball grid array) welding columns and a preparation method thereof.
Background
Ball Grid Array (BGA) technology is a surface mount technology applied to integrated circuits, and as the IC packaging technology is developed to high density, thin, high performance and low cost, BGA is increasingly used in the fields of military industry, aviation, aerospace, etc. due to its high reliability and excellent electrical and thermal properties.
The CCGA is used as a packaging form of the BGA, the packaging structure is an integrated circuit chip in a top mode of a ceramic substrate, and is mostly in a flip-chip mode, and compared with a traditional packaging form, the CCGA does not use a solder ball connected below the ceramic substrate, but a 90Sn/10Pb welding column, and has higher assembly reliability.
PCBA, i.e., printed circuit board assembly, refers to the mounting and soldering of CCGA devices to a Printed Circuit Board (PCB) by means of Surface Mount Technology (SMT) or interposer technology (THT), etc., to form an electronic device with specific functions, the technology used being also called chip technology. In short, PCBA is an electronic module in which various electronic components are mounted on a printed circuit board.
In the practical application process, the welding column of the CCGA device is found to be about 20% -30% reduced in shock resistance and shear strength after being subjected to temperature cycle, high-low temperature storage and other reliability tests; in the thermal shock test, failure fracture phenomenon still occurs at the welding interface of the welding column and the substrate and at the end part of the welding column wrapped by the welding flux. Therefore, the BGA solder columns are generally required to be reinforced, and the current reinforcement methods are broadly divided into two types: an epoxy resin adhesive is adopted, a proper amount of epoxy resin adhesive is filled along the periphery of a CCGA device, and the epoxy resin adhesive is cured in a heating furnace or an oven under the high temperature condition; the other is to coat the periphery of the CCGA device by adopting a UV curing material, and to cure the CCGA device by UV irradiation in a UV furnace or an ultraviolet device such as an LED area light source; thereby improving the reliability and lifetime of BGA solder columns.
The epoxy resin adhesive is widely used because of simple use and operation, excellent strength and impact resistance after curing and better adhesion; however, the capability of resisting cold and hot changes is weak, after the cold and hot impact, the structural strength of the steel plate is reduced, cracks are easily generated, the reinforcing effect is reduced, the overall service life is reduced, and the use stability of the final product is further affected, so that a scheme is required to be provided at present so as to solve the technical problems.
Disclosure of Invention
In order to improve the reinforcement stability of the epoxy resin adhesive to the BGA welding column in a cold and hot change environment, the application provides the epoxy resin adhesive for reinforcing the BGA welding column.
In a first aspect, the application provides an epoxy adhesive for reinforcing a BGA solder post, which adopts the following technical scheme:
the epoxy adhesive for reinforcing the BGA welding column comprises an A component and a B component, wherein the A component comprises the following raw materials in parts by weight:
70-80 parts of bisphenol A type epoxy resin;
5-10 parts of carboxyl-terminated liquid nitrile rubber;
2-5 parts of polysulfide rubber;
3-7 parts of nano alumina whisker;
1-5 parts of a silane coupling agent;
10-15 parts of reactive diluent;
3-5 parts of filler;
the component B consists of the following raw materials in parts by weight:
70-90 parts of curing agent;
2-6 parts of a promoter;
the weight ratio of the component A to the component B is (2.2-3.8) 1.
By adopting the technical scheme, the use of the polysulfide rubber changes the crosslinking density of the epoxy adhesive system through the chain length of the self molecules, reduces the curing stress of the system, increases the movement capability between the crosslinking points of the resin network, and when cracks are generated in a matrix, the expansion direction of the cracks is easy to change and bend, so that the cracks are not easy to generate; the carboxyl-terminated liquid nitrile rubber can become a disperse phase in a continuous phase formed by an epoxy resin crosslinked network, and dispersed phase particles form a sea-island structure, so that the internal stress change can be well regulated and controlled; the nano aluminum oxide whisker is uniformly dispersed in the epoxy adhesive system, and can bring inhibition effect to crack expansion by forming an effect larger than Van der Waals force on an interface with an epoxy group. Meanwhile, excellent compounding effect can be achieved among the carboxyl-terminated liquid nitrile rubber, the polysulfide rubber and the nano aluminum oxide whisker, after the cured epoxy rubber is subjected to cold and hot impact, microcracks generated in the cured epoxy rubber are led to the nano aluminum oxide whisker through the polysulfide rubber, at the moment, most of microcracks are prevented from expanding and ending, and the expansion of residual microcracks can be further prevented by leading the nano aluminum oxide whisker into disperse phase particles formed by the carboxyl-terminated liquid nitrile rubber; therefore, the crack resistance of the epoxy adhesive for reinforcing the BGA welding column in a cold and hot changing environment can be obviously improved, and the reliability and the service life of the BGA welding column are further improved.
Preferably, the weight ratio of the component A to the component B is 3:1.
By adopting the technical scheme, after the component A and the component B in the weight ratio are mixed, a relatively excellent and stable curing effect can be obtained, and particularly, the epoxy glue can better cope with the expansion of microcracks in a cold and hot changing environment aiming at the matching of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano aluminum oxide whisker in an epoxy glue system, so that the reliability and the service life of the obtained epoxy glue for reinforcing the BGA welding column after being applied in the cold and hot changing environment are relatively outstanding.
Preferably, the diameter of the nano alumina whisker is 5-10nm, and the length is 50-200nm.
By adopting the technical scheme, in the resin system of the planned nano aluminum oxide whisker which can be uniformly dispersed and epoxy glue, when the cured epoxy glue is subjected to cold and hot impact, the nano aluminum oxide whisker has higher bearing effect on the expansion of microcracks, and after bearing, the nano aluminum oxide whisker is inhibited or guided into dispersed phase particles formed by carboxyl-terminated liquid nitrile rubber, so that the microcracks can be obviously prevented from being expanded to form cracks, and the obtained epoxy glue for reinforcing the BGA welding column has higher product performance in the application of cold and hot change environment.
Preferably, the weight ratio of the carboxyl-terminated liquid nitrile rubber to the polysulfide rubber to the nano aluminum oxide whisker is 8:3:5.
By adopting the technical scheme, the compound effect of the carboxyl-terminated liquid nitrile rubber, the polysulfide rubber and the nano aluminum oxide whisker in the epoxy adhesive system is excellent, the micro cracks generated under cold and hot impact are treated with high rate, the micro cracks can be effectively prevented from being converted into cracks, and the obtained epoxy adhesive for reinforcing the BGA welding column has high quality.
Preferably, the epoxy equivalent of the bisphenol A type epoxy resin is 250-450g/eq, and the molecular weight of the carboxyl-terminated liquid nitrile rubber is 6000-8000.
By adopting the technical scheme, the bisphenol A epoxy resin with the epoxy equivalent has strong adhesive force, excellent electrical insulation performance and low molecular weight epoxy resin, and is more suitable for reinforcing BGA welding columns; the bisphenol A type epoxy resin and the carboxyl-terminated liquid nitrile rubber with the specifications are matched, so that dispersed phase particles formed by the carboxyl-terminated liquid nitrile rubber in an epoxy resin cross-linked network are more uniform, and further, excellent matching effects are exerted between the carboxyl-terminated liquid nitrile rubber and polysulfide rubber as well as between the carboxyl-terminated liquid nitrile rubber and nano aluminum oxide whiskers, and the epoxy rubber for reinforcing the BGA welding column can be obtained, wherein the epoxy rubber is more stable and durable in application in cold and hot changing environments.
Preferably, the reactive diluent is any one or a combination of a plurality of butyl glycidyl ether, glycerol epoxy resin, resorcinol diglycidyl ether, phenyl glycidyl ether and cresol glycidyl ether.
By adopting the technical scheme, the molecular structure of the reactive diluent contains the active groups, so that the reactive diluent can participate in the curing and crosslinking reaction of epoxy, and the overall performance of the epoxy adhesive for reinforcing the BGA welding column after curing is improved; meanwhile, the reactive diluent can adjust the fluidity of the epoxy adhesive for reinforcing the BGA welding column, and is easier to coat and adhere in the use process; the reactive diluents of the above types can be stably applied to the epoxy glue for reinforcing the BGA solder columns, and exert excellent stabilizing effect.
Preferably, the filler is any one or a combination of a plurality of wollastonite, calcium silicate, quartz powder, asbestos powder, talcum powder and graphite powder.
By adopting the technical scheme, the filler of the type can be uniformly dispersed among the raw materials of all the components, so that the viscosity of the epoxy adhesive for reinforcing the BGA welding column and the strength after curing are improved and stably ensured, and the epoxy adhesive for reinforcing the BGA welding column with excellent quality can be obtained.
Preferably, the curing agent is a polyetheramine curing agent.
Through adopting above-mentioned technical scheme, polyether amine curing agent's reactivity is high, solidification speed is fast, stable performance, in the solidification process of the epoxy glue for BGA welding post reinforcement, can make each component raw materials fully combine the effect, and the stability of the solidification structure of formation in cold and hot change environment is comparatively excellent, and whole life is longer.
Preferably, the accelerator is any one or a combination of a plurality of triethanolamine, aniline, benzoate, phenylacetate, acetic anhydride and acrylic anhydride.
By adopting the technical scheme, the accelerators of the types can accelerate the curing and crosslinking process, so that the epoxy adhesive for reinforcing the BGA welding column can be cured more rapidly after being applied, and the reinforcing of the welding column is more suitable; meanwhile, the accelerator can also effectively increase the binding force among the raw materials of all the components, so that the epoxy adhesive for reinforcing the BGA welding column is more stable and reliable in the bonding process.
In a second aspect, the application provides a preparation method of epoxy glue for reinforcing a BGA solder post, which adopts the following technical scheme:
the preparation method of the epoxy adhesive for reinforcing the BGA welding column comprises the following steps:
(1) Preparing raw materials comprising bisphenol A epoxy resin, carboxyl-terminated liquid nitrile rubber, polysulfide rubber, nano aluminum oxide whisker, silane coupling agent, reactive diluent, filler, curing agent and accelerator according to a proportion;
(2) Uniformly stirring and mixing bisphenol A type epoxy resin, carboxyl-terminated liquid nitrile rubber, polysulfide rubber, nano aluminum oxide whisker, a silane coupling agent, a reactive diluent and a filler in the step (1) to obtain a component A mixture; uniformly stirring and mixing the curing agent and the accelerator in the step (1) to obtain a component B mixture;
(3) And (3) uniformly mixing the component A mixture and the component B mixture in the step (2) according to the corresponding weight ratio to obtain the epoxy adhesive for reinforcing the BGA welding column.
By adopting the technical scheme, the component A and the component B are respectively and uniformly mixed, and then mixed according to the proportion, so that the obtained epoxy adhesive for reinforcing the BGA welding column can be directly used; meanwhile, the prepared A component mixture and B component mixture can be respectively and independently filled and stored, and can be mixed when in use, so that the whole is more convenient and quick.
In summary, the present application has the following beneficial effects:
1. according to the epoxy resin adhesive, the carboxyl-terminated liquid nitrile rubber, the polysulfide rubber and the nano aluminum oxide whisker are compounded in the epoxy resin adhesive, after the cured epoxy resin adhesive is subjected to cold and hot impact, microcracks generated in the cured epoxy resin adhesive and the expansion of the microcracks can be effectively inhibited, so that the microcracks can be effectively avoided, and the epoxy resin adhesive for reinforcing the BGA welding columns has excellent and remarkable reinforcing stability; 2. the specification of bisphenol A type epoxy resin, carboxyl-terminated liquid nitrile rubber and nano alumina whisker is further limited, so that the epoxy resin plays a better role in the application process, and cracks formed by micro crack expansion can be remarkably avoided, so that the obtained epoxy resin for reinforcing the BGA welding column has excellent applicability in cold and hot change environments and has better overall quality.
Detailed Description
The present application is described in further detail below with reference to examples.
The raw materials used in the preparation examples and examples of the present application are all commercially available except for the specific descriptions:
bisphenol a epoxy resins are available from wuhan gold sources and chemical industry limited;
the carboxyl-terminated liquid nitrile rubber was purchased from atanan macro Cheng Di new materials limited;
polysulfide rubber was purchased from Kang Disi chemical (Hubei) Co., ltd., CAS number 63148-67-4;
the silane coupling agent is KH-560;
polyetheramine curing agent is available from polyetheramine ED600 epoxy curing agent of Jieshikari, inc. of Wuhan Hua Xiangke.
Examples
Example 1
The epoxy adhesive for reinforcing the BGA welding column comprises an A component and a B component, wherein the raw materials of the A component and the B component and the corresponding weights of the raw materials are shown in a table 1, and the epoxy adhesive is prepared by the following steps:
(1) Preparing raw materials comprising bisphenol A epoxy resin, carboxyl-terminated liquid nitrile rubber, polysulfide rubber, nano aluminum oxide whisker, silane coupling agent, reactive diluent, filler, curing agent and accelerator according to a proportion;
(2) Uniformly stirring and mixing bisphenol A type epoxy resin, carboxyl-terminated liquid nitrile rubber, polysulfide rubber, nano aluminum oxide whisker, a silane coupling agent, an active diluent and a filler in the step (1), and stirring at 1200rpm for 70min to obtain a component A mixture; uniformly stirring and mixing the curing agent and the accelerator in the step (1), and stirring at 500rpm for 20min to obtain a component B mixture;
(3) And (3) uniformly mixing the component A mixture and the component B mixture in the step (2) according to the corresponding weight ratio, and stirring at 1000rpm for 10min to obtain the epoxy glue for reinforcing the BGA welding column.
Note that: in the operation, the weight ratio of the component A to the component B is 3:1; the diameter of the nano alumina whisker is 7.5nm, and the length is 125nm; the epoxy equivalent of the bisphenol A epoxy resin is 350g/eq, and the molecular weight of the carboxyl-terminated liquid nitrile rubber is 7000; the curing agent is polyether amine curing agent; the reactive diluent is butyl glycidyl ether; the filler particle size is silicon 10um, wollastonite in this example; the promoter is triethanolamine.
Examples 2 to 3
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the raw materials of the A component and the B component and the corresponding weights thereof are shown in Table 1.
Table 1 raw materials for the A component and the B component in examples 1 to 3 and parts by weight (kg/part)
Example 4
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the weight ratio of the component A to the component B is 2.2:1.
Example 5
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the weight ratio of the component A to the component B is 3.8:1.
Example 6
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the weight ratio of the component A to the component B is 3.1:1.
Example 7
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the weight ratio of the component A to the component B is 2.9:1.
Example 8
The epoxy glue for reinforcing BGA solder columns is different from the epoxy glue in the embodiment 1 in that the diameter of the nano alumina whisker is 5nm and the length is 50nm.
Example 9
The epoxy glue for reinforcing BGA solder columns is different from the epoxy glue in the embodiment 1 in that the diameter of the nano alumina whisker is 10nm and the length is 200nm.
Example 10
The epoxy glue for reinforcing BGA solder columns is different from the epoxy glue in the embodiment 1 in that the diameter of the nano alumina whisker is 4.5nm and the length is 45nm.
Example 11
The epoxy glue for reinforcing BGA solder columns is different from the epoxy glue in the embodiment 1 in that the diameter of the nano alumina whisker is 10.5nm and the length is 205nm.
Example 12
An epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the epoxy equivalent of bisphenol A type epoxy resin is 250g/eq and the molecular weight of carboxyl terminated liquid nitrile rubber is 6000.
Example 13
An epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the epoxy equivalent of bisphenol A type epoxy resin is 450g/eq and the molecular weight of carboxyl terminated liquid nitrile rubber is 8000.
Example 14
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the epoxy equivalent of bisphenol A type epoxy resin is 200g/eq and the molecular weight of carboxyl terminated liquid nitrile rubber is 5500.
Example 15
An epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the epoxy equivalent of bisphenol A type epoxy resin is 500g/eq and the molecular weight of carboxyl terminated liquid nitrile rubber is 8500.
Example 16
The epoxy adhesive for reinforcing BGA solder columns is different from the epoxy adhesive in example 1 in that the reactive diluent is a composition of resorcinol diglycidyl ether and phenyl glycidyl ether in a weight ratio of 1:1.
Example 17
The epoxy adhesive for reinforcing BGA solder columns is different from the epoxy adhesive in the embodiment 1 in that the filler is a composition of quartz powder and talcum powder according to a weight ratio of 1:1.
Example 18
The epoxy adhesive for reinforcing BGA solder columns is different from the epoxy adhesive in example 1 in that the accelerator is a composition of triethanolamine and benzoate in a weight ratio of 1:1.
Example 19
The epoxy adhesive for reinforcing BGA welding columns is different from the epoxy adhesive in the embodiment 1 in that the total weight of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano aluminum oxide whisker is unchanged, and the weight ratio of the carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano aluminum oxide whisker is adjusted to be 8:3:5.
Example 20
An epoxy adhesive for reinforcing BGA solder columns is different from example 19 in that the weight ratio of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano alumina whiskers is 7.8:3:5.
Example 21
An epoxy adhesive for reinforcing BGA solder columns is different from example 19 in that the weight ratio of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano alumina whiskers is 8.2:3:5.
Example 22
An epoxy adhesive for reinforcing BGA solder columns is different from example 19 in that the weight ratio of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano alumina whisker is 8:2.8:5.
Example 23
An epoxy adhesive for reinforcing BGA solder columns is different from example 19 in that the weight ratio of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano alumina whisker is 8:3.2:5.
Example 24
The epoxy adhesive for reinforcing BGA solder columns is different from example 19 in that the weight ratio of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano aluminum oxide whisker is 8:3:5.2.
Example 25
The epoxy adhesive for reinforcing BGA solder columns is different from example 19 in that the weight ratio of carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano aluminum oxide whisker is 8:3:4.8.
Comparative example
Comparative example 1
The epoxy adhesive for reinforcing BGA solder columns is different from that of example 1 in that the raw materials do not contain carboxyl-terminated liquid nitrile rubber and nano alumina whisker.
Comparative example 2
The epoxy glue for reinforcing BGA solder columns is different from that of example 1 in that the raw material does not contain polysulfide rubber and nano alumina whisker.
Comparative example 3
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the raw material does not contain carboxyl-terminated liquid nitrile rubber and polysulfide rubber.
Comparative example 4
The epoxy glue for reinforcing BGA solder columns is different from that of example 1 in that the raw material does not contain nano alumina whisker.
Comparative example 5
An epoxy adhesive for reinforcing BGA solder columns is different from that of example 1 in that polysulfide rubber is not contained in the raw material.
Comparative example 6
An epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the raw material does not contain carboxyl-terminated liquid nitrile rubber.
Comparative example 7
The epoxy adhesive for reinforcing BGA solder columns is different from example 1 in that the raw materials do not contain carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano alumina whisker.
Performance test samples: the BGA post-reinforcement epoxy adhesives obtained in examples 1 to 25 were used as test samples 1 to 25, and the BGA post-reinforcement epoxy adhesives obtained in comparative examples 1 to 7 were used as control samples 1 to 7.
The test method comprises the following steps: test samples 1 to 25 and control samples 1 to 7 were tested according to GB/T2423.22-2012 environmental test part 2: test method test N: temperature variation testing, -40 ℃/8h-85 ℃/8h, then placing at 95% relative humidity and 85 ℃ for 24h, wherein the above is one cycle of high-low temperature cycle treatment, each environment is switched within 2min, and the cycle is completed for 30 times, thus completing the high-low temperature cycle test; at the beginning of the test, using a tearing strength tester to obtain the tearing strength corresponding to the test samples 1-25 and the control samples 1-7, and marking the tearing strength as initial tearing strength, and after the high-low temperature cycle test is completed, obtaining the tearing strength by the same method, and marking the tearing strength as the tearing strength after the cycle; finally, the tear strength decay rate (%), tear strength decay rate= (initial tear strength-tear strength after cycling)/initial tear strength was calculated. The higher the tearing strength attenuation rate is, the worse the cold and hot impact resistance of the epoxy adhesive for reinforcing the BGA welding column is, the more microcracks are formed in the epoxy adhesive, the more serious the microcracks are expanded, and the epoxy adhesive is easy to tear.
TABLE 2 test results for test samples 1-25 and control samples 1-7
As can be seen by combining the example 1 and the comparative examples 1-7 and combining the table 2, the carboxyl-terminated liquid nitrile rubber, polysulfide rubber and nano alumina whisker can play an excellent role in compounding, so that the epoxy adhesive for reinforcing the BGA welding column has excellent cold and hot impact resistance, and the tearing strength attenuation rate obtained by testing is obviously lower; any one of the carboxyl-terminated liquid nitrile rubber, the polysulfide rubber and the nano aluminum oxide whisker is singly used, or any two of the carboxyl-terminated liquid nitrile rubber, the polysulfide rubber and the nano aluminum oxide whisker are combined for use, so that the improvement on the cold and hot impact resistance of the epoxy adhesive is limited, and the effect exerted by the compounding of the three is far less excellent.
As can be seen from the combination of examples 1 and examples 4 to 7 and the combination of table 2, when the weight ratio of the component a to the component B is 3:1, the stability of the epoxy adhesive for reinforcing BGA solder columns after application in a cold and hot changing environment is excellent, and the tear strength attenuation rate obtained by the test is also significantly lower, which is based on the curing at this ratio, and is more favorable for the excellent effect of carboxyl terminated liquid nitrile rubber, polysulfide rubber and nano-alumina whiskers in an epoxy adhesive system.
As can be seen from the combination of the examples 1 and 8-11 and the Table 2, the nano alumina whisker has a diameter of 5-10nm and a length of 50-200nm, and has a stable and excellent effect in application, and has a good matching effect with carboxyl-terminated liquid nitrile rubber and polysulfide rubber, and the obtained epoxy adhesive for reinforcing BGA welding columns has excellent cold and heat impact resistance. When the particle size exceeds the above specification range, the tear strength attenuation rate is obviously increased, and the particle size is too small to be uniformly dispersed, and when the particle size is too large, the connection between dispersed phase particles formed by the particle size and the carboxyl-terminated liquid nitrile rubber is poor, so that the cold and hot impact resistance is reduced.
As can be seen from the combination of examples 1 and 12-15 and the combination of table 2, the epoxy equivalent of bisphenol a type epoxy resin is 250-450g/eq, and the molecular weight of the carboxyl-terminated liquid nitrile rubber is 6000-8000, so that the epoxy adhesive for reinforcing the BGA solder columns can have excellent and stable cold and heat impact resistance; and beyond the specification requirements, the performance of the epoxy adhesive for reinforcing the BGA solder columns is poorer than that of the epoxy adhesive for reinforcing the BGA solder columns obviously.
As can be seen from the combination of the examples 1 and 19-25 and the table 2, the weight ratio of the carboxyl-terminated liquid nitrile rubber to the polysulfide rubber to the nano aluminum oxide whisker is 8:3:5, the effect brought by the mutual cooperation is more excellent, the inhibition rate of microcracks generated under cold and hot impact is higher, the microcracks can be effectively prevented from being converted into cracks, and the epoxy adhesive for reinforcing the BGA welding column with higher quality can be obtained.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (8)
1. The epoxy adhesive for reinforcing the BGA welding column is characterized by comprising an A component and a B component, wherein the A component consists of the following raw materials in parts by weight:
70-80 parts of bisphenol A type epoxy resin;
5-10 parts of carboxyl-terminated liquid nitrile rubber;
2-5 parts of polysulfide rubber;
3-7 parts of nano alumina whisker;
1-5 parts of a silane coupling agent;
10-15 parts of reactive diluent;
3-5 parts of filler;
the component B consists of the following raw materials in parts by weight:
70-90 parts of curing agent;
2-6 parts of a promoter;
the weight ratio of the component A to the component B is (2.2-3.8) 1;
the diameter of the nano alumina whisker is 5-10nm, and the length is 50-200nm;
the epoxy equivalent of the bisphenol A type epoxy resin is 250-450g/eq, and the molecular weight of the carboxyl-terminated liquid nitrile rubber is 6000-8000.
2. The epoxy glue for reinforcing a BGA solder post according to claim 1, wherein: the weight ratio of the component A to the component B is 3:1.
3. The epoxy glue for reinforcing a BGA solder post according to claim 1, wherein: the weight ratio of the carboxyl-terminated liquid nitrile rubber to the polysulfide rubber to the nanometer alumina whisker is 8:3:5.
4. The epoxy glue for reinforcing a BGA solder post according to claim 1, wherein: the reactive diluent is any one or a combination of a plurality of butyl glycidyl ether, glycerol epoxy resin, resorcinol diglycidyl ether, phenyl glycidyl ether and cresol glycidyl ether.
5. The epoxy glue for reinforcing a BGA solder post according to claim 1, wherein: the filler is any one or a combination of more of wollastonite, calcium silicate, quartz powder, asbestos powder, talcum powder and graphite powder.
6. The epoxy glue for reinforcing a BGA solder post according to claim 1, wherein: the curing agent is polyether amine curing agent.
7. The epoxy glue for reinforcing a BGA solder post according to claim 1, wherein: the promoter is any one or a combination of a plurality of triethanolamine, aniline, benzoate, phenylacetate, acetic anhydride and acrylic anhydride.
8. The method for preparing the epoxy adhesive for reinforcing the BGA solder columns, as set forth in claim 1, is characterized in that: the method comprises the following steps:
(1) Preparing raw materials comprising bisphenol A epoxy resin, carboxyl-terminated liquid nitrile rubber, polysulfide rubber, nano aluminum oxide whisker, silane coupling agent, reactive diluent, filler, curing agent and accelerator according to a proportion;
(2) Uniformly stirring and mixing bisphenol A type epoxy resin, carboxyl-terminated liquid nitrile rubber, polysulfide rubber, nano aluminum oxide whisker, a silane coupling agent, a reactive diluent and a filler in the step (1) to obtain a component A mixture; uniformly stirring and mixing the curing agent and the accelerator in the step (1) to obtain a component B mixture;
(3) And (3) uniformly mixing the component A mixture and the component B mixture in the step (2) according to the corresponding weight ratio to obtain the epoxy adhesive for reinforcing the BGA welding column.
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