CN110760284A - Composite Ag conductive adhesive capable of effectively controlling Ag ion migration - Google Patents
Composite Ag conductive adhesive capable of effectively controlling Ag ion migration Download PDFInfo
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- CN110760284A CN110760284A CN201910972583.7A CN201910972583A CN110760284A CN 110760284 A CN110760284 A CN 110760284A CN 201910972583 A CN201910972583 A CN 201910972583A CN 110760284 A CN110760284 A CN 110760284A
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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
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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
- 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
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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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Conductive Materials (AREA)
Abstract
The invention relates to the technical field of composite conductive adhesives, and discloses a composite Ag conductive adhesive for effectively controlling Ag ion migration, which comprises the following raw materials in parts by weight: 100 parts of epoxy resin E-51 matrix resin, 98 parts of curing agent, 0.67 part of curing accelerator, 6-10 parts of sodium dimercaptopropanesulfonate and 6-14 parts of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver powder coating comprises a composite type surfactant, 140-165 parts of silver powder conductive filler, 2 parts of silane coupling agent, 1 part of antioxidant and 2 parts of defoaming agent. The invention solves the technical problem that the connection reliability of the conductive adhesive is reduced because Ag ions are easy to migrate in the use process of the existing composite Ag conductive adhesive.
Description
Technical Field
The invention relates to the technical field of composite conductive adhesives, in particular to a composite Ag conductive adhesive for effectively controlling Ag ion migration.
Background
With the development of microelectronic assembly industry towards high density and high integration and stricter environmental legislation, it is imperative that conductive adhesives replace soldering lead solder in the field of microelectronic assembly. The conductive adhesive is classified into two types, one is an intrinsic conductive adhesive, which is a conjugated polymer with a molecular structure having a conductive function, and is mostly composed of a polyphenylene and polyacetylene-based compound, and the other is a composite conductive adhesive in which conductive particles are filled in the polymer.
The composite conductive adhesive generally comprises a matrix resin, a curing agent, a curing accelerator, a diluent, conductive particles and other additives. At present, silver is the most used conductive particle in the composite conductive adhesive, and under the action of moisture and high-density current, because of high solubility and low migration excitation energy of silver ions, dendritic crystals are easy to form and a stable passivation film is difficult to form, so that the silver is easier to migrate compared with other metals.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a composite Ag conductive adhesive for effectively controlling Ag ion migration, so as to solve the technical problem that the connection reliability of the conductive adhesive is reduced because Ag ion migration is easy to occur in the use process of the existing composite Ag conductive adhesive.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a composite Ag conductive adhesive for effectively controlling Ag ion migration comprises the following raw materials in parts by weight: 100 parts of epoxy resin E-51 matrix resin, 98 parts of curing agent, 0.67 part of curing accelerator, 6-10 parts of sodium dimercaptopropanesulfonate and 6-14 parts of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver powder coating comprises a composite type surfactant, 140-165 parts of silver powder conductive filler, 2 parts of silane coupling agent, 1 part of antioxidant and 2 parts of defoaming agent.
Further, the average grain diameter of the silver powder conductive filler is less than or equal to 7 um.
Further, the composite Ag conductive adhesive comprises the following raw materials in parts by weight: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, 8g of sodium dimercaptopropanesulfonate and 12g of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver-aluminum alloy wire material comprises a composite type surfactant, 140g of silver powder conductive filler with the average grain diameter less than or equal to 7um, 2g of r-aminopropyl triethoxysilane coupling agent, 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent.
Further, the composite Ag conductive adhesive comprises the following raw materials in parts by weight: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, a mixture of 6g of sodium dimercaptopropanesulfonate and 14g of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver-aluminum alloy wire material comprises a composite type surfactant, 140g of silver powder conductive filler with the average grain diameter less than or equal to 7um, 2g of r-aminopropyl triethoxysilane coupling agent, 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the resin is prepared by adding 6-10 parts of sodium dimercaptopropanesulfonate and 6-14 parts of 3-hydroxypropanetricarboxylic acid (H) into a resin matrix3C6H5O7) The composite type surfactant and 140-165 parts of silver powder conductive filler are ground and mixed to prepare the composite Ag conductive adhesive;
the silver powder conductive filler is subjected to surface treatment by using the composite surfactant to generate a chelate monomolecular film so as to improve the Ag ion migration resistance of the conductive adhesive;
the contact resistance of the composite Ag conductive adhesive prepared by the invention after aging in an aging environment of 85 ℃/85% RH is 0.07-0.14 omega, and the tensile strength change rate is 4.61-6.32%;
compared with the contact resistance of 0.56 omega and the tensile strength change rate of 21.8 percent of the composite Ag conductive adhesive prepared by the comparative example after aging in the aging environment of 85 ℃/85 percent RH, the contact resistance of the composite Ag conductive adhesive after aging in the aging environment of 85 ℃/85 percent RH is obviously reduced, and the tensile strength change rate of the composite Ag conductive adhesive after aging in the aging environment of 85 ℃/85 percent RH is obviously reduced, so that the technical effect of obviously improving the connection reliability of the conductive adhesive is achieved;
therefore, the technical problem that the connection reliability of the conductive adhesive is reduced because Ag ions are easy to migrate in the using process of the existing composite Ag conductive adhesive is solved.
Detailed Description
The following raw materials were used:
epoxy resin E-51, the epoxy equivalent is 185-208 g/eq, the epoxy value is 0.48-0.54 eq/100g, and the viscosity is less than or equal to 2.5 Pa.s (at 25 ℃);
methylhexahydrophthalic anhydride (MeHHPA), acid number 657.32, free acid 0.18%, iodine number 0.87, freezing point-15 ℃.
The first embodiment is as follows:
the composite Ag conductive adhesive comprises the following raw materials in parts by weight: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, a mixture of 10g of sodium dimercaptopropanesulfonate and 6g of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver-silicon composite material comprises a composite type surfactant, 140g of silver powder conductive filler with the average grain diameter less than or equal to 7um, 2g of r-aminopropyl triethoxysilane coupling agent, 1g of phenyl hydroquinone antioxidant and 2g of organosilicon compound defoaming agent;
the preparation method of the composite Ag conductive adhesive comprises the following steps:
the method comprises the following steps: weighing 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent and 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator in sequence into a beaker, stirring for 10min to uniformly mix the components of the matrix, vacuumizing for 30min to remove bubbles, and preparing to obtain a resin matrix;
step two: the resin matrix prepared above was transferred to an agate mortar, and 10g of sodium dimercaptopropanesulfonate and 6g of 3-hydroxypropanetricarboxylic acid (H) were added to the agate mortar3C6H5O7) Grinding the composite surfactant until the composite surfactant is uniform;
step three: adding 40g of silver powder conductive filler into an agate mortar for the first time, and grinding for 5 min; then adding 1g of malonic acid conduction promoter and 2g of r-aminopropyltriethoxysilane coupling agent, and grinding until the mixture is uniform;
step four: adding 100g of silver powder conductive filler into the agate mortar for the second time, and grinding for 15 min; then adding 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent, and grinding for 15min to prepare the composite Ag conductive adhesive.
Example two:
the composite Ag conductive adhesive comprises the following components in parts by weightThe raw materials in proportion by weight are as follows: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, 8g of sodium dimercaptopropanesulfonate and 12g of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver-silicon composite material comprises a composite type surfactant, 140g of silver powder conductive filler with the average grain diameter less than or equal to 7um, 2g of r-aminopropyl triethoxysilane coupling agent, 1g of phenyl hydroquinone antioxidant and 2g of organosilicon compound defoaming agent;
the preparation method of the composite Ag conductive adhesive comprises the following steps:
the method comprises the following steps: weighing 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent and 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator in sequence into a beaker, stirring for 10min to uniformly mix the components of the matrix, vacuumizing for 30min to remove bubbles, and preparing to obtain a resin matrix;
step two: the resin matrix prepared above was transferred to an agate mortar, and 8g of sodium dimercaptopropanesulfonate and 12g of 3-hydroxypropanetricarboxylic acid (H) were added to the agate mortar3C6H5O7) Grinding the composite surfactant until the composite surfactant is uniform;
step three: adding 50g of silver powder conductive filler into an agate mortar for the first time, and grinding for 5 min; then adding 1g of malonic acid conduction promoter and 2g of r-aminopropyltriethoxysilane coupling agent, and grinding until the mixture is uniform;
step four: adding 100g of silver powder conductive filler into the agate mortar for the second time, and grinding for 15 min; then adding 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent, and grinding for 15min to prepare the composite Ag conductive adhesive.
Example three:
the composite Ag conductive adhesive comprises the following raw materials in parts by weight: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, a mixture of 6g of sodium dimercaptopropanesulfonate and 14g of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver-silicon composite material comprises a composite type surfactant, 140g of silver powder conductive filler with the average grain diameter less than or equal to 7um, 2g of r-aminopropyl triethoxysilane coupling agent, 1g of phenyl hydroquinone antioxidant and 2g of organosilicon compound defoaming agent;
the preparation method of the composite Ag conductive adhesive comprises the following steps:
the method comprises the following steps: weighing 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent and 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator in sequence into a beaker, stirring for 10min to uniformly mix the components of the matrix, vacuumizing for 30min to remove bubbles, and preparing to obtain a resin matrix;
step two: the resin matrix prepared above was transferred to an agate mortar, and 6g of sodium dimercaptopropanesulfonate and 14g of 3-hydroxypropanetricarboxylic acid (H) were added to the agate mortar3C6H5O7) Grinding the composite surfactant until the composite surfactant is uniform;
step three: adding 65g of silver powder conductive filler into an agate mortar for the first time, and grinding for 5 min; then adding 1g of malonic acid conduction promoter and 2g of r-aminopropyltriethoxysilane coupling agent, and grinding until the mixture is uniform;
step four: adding 100g of silver powder conductive filler into the agate mortar for the second time, and grinding for 15 min; then adding 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent, and grinding for 15min to prepare the composite Ag conductive adhesive.
Comparative example:
the composite Ag conductive adhesive comprises the following raw materials in parts by weight: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, 150g of silver powder conductive filler with the average particle size of less than or equal to 7um, 2g of r-aminopropyltriethoxysilane coupling agent, 1g of phenylhydroquinone antioxidant and 2g of organosilicon compound defoaming agent;
the preparation method of the composite Ag conductive adhesive comprises the following steps:
the method comprises the following steps: weighing 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent and 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator in sequence into a beaker, stirring for 10min to uniformly mix the components of the matrix, vacuumizing for 30min to remove bubbles, and preparing to obtain a resin matrix;
step two: transferring the prepared resin matrix into an agate mortar, and grinding the resin matrix to be uniform;
step three: adding 50g of silver powder conductive filler into an agate mortar for the first time, and grinding for 5 min; then 2g of r-aminopropyl triethoxysilane coupling agent is added, and the mixture is ground to be uniform;
step four: adding 100g of silver powder conductive filler into the agate mortar for the second time, and grinding for 15 min; then adding 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent, and grinding for 15min to prepare the composite Ag conductive adhesive.
And (3) performance testing:
after the composite Ag conductive adhesive prepared in the above examples and comparative examples is placed in an aging environment at 85 ℃/85% RH for 20 days, the contact resistance of the conductive adhesive is tested, and the test results are shown in Table 1;
the tensile strength of the composite Ag conductive adhesives prepared in the above examples and comparative examples was tested, and then the composite Ag conductive adhesives were left in an aging environment at 85 ℃/85% RH for 20 days, and then the tensile strength was tested, and the test results are shown in table 1.
TABLE 1
Claims (4)
1. The composite Ag conductive adhesive for effectively controlling Ag ion migration is characterized by comprising the following raw materials in parts by weight: 100 parts of epoxy resin E-51 matrix resin, 98 parts of curing agent, 0.67 part of curing accelerator, 6-10 parts of sodium dimercaptopropanesulfonate and 6-14 parts of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) Composite surfactant140-165 parts of silver powder conductive filler, 2 parts of silane coupling agent, 1 part of antioxidant and 2 parts of defoaming agent.
2. The composite Ag conductive adhesive according to claim 1, wherein the silver powder conductive filler has an average particle size of 7um or less.
3. The composite Ag conductive adhesive according to claim 2, wherein the composite Ag conductive adhesive comprises the following raw materials in parts by weight: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, 8g of sodium dimercaptopropanesulfonate and 12g of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver-aluminum alloy wire material comprises a composite type surfactant, 140g of silver powder conductive filler with the average grain diameter less than or equal to 7um, 2g of r-aminopropyl triethoxysilane coupling agent, 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent.
4. The composite Ag conductive adhesive according to claim 3, wherein the composite Ag conductive adhesive comprises the following raw materials in parts by weight: 100g of epoxy resin E-51 matrix resin, 98g of methylhexahydrophthalic anhydride (MeHHPA) curing agent, 0.67g of 2-ethyl-4-methylimidazole (2E4MZ) curing accelerator, a mixture of 6g of sodium dimercaptopropanesulfonate and 14g of 3-hydroxypropanetricarboxylic acid (H)3C6H5O7) The composite type silver-aluminum alloy wire material comprises a composite type surfactant, 140g of silver powder conductive filler with the average grain diameter less than or equal to 7um, 2g of r-aminopropyl triethoxysilane coupling agent, 1g of phenyl hydroquinone antioxidant and 2g of organic silicon compound defoaming agent.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115746762A (en) * | 2022-11-28 | 2023-03-07 | 北京化工大学 | Low-migration high-conductivity silver adhesive and preparation method thereof |
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2019
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JP2893782B2 (en) * | 1990-01-19 | 1999-05-24 | 日立化成工業株式会社 | Conductive adhesive and semiconductor device |
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Cited By (1)
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CN115746762A (en) * | 2022-11-28 | 2023-03-07 | 北京化工大学 | Low-migration high-conductivity silver adhesive and preparation method thereof |
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