CN110003833A - A kind of preparation method of SMT Heraeus - Google Patents
A kind of preparation method of SMT Heraeus Download PDFInfo
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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
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The present invention relates to a kind of preparation methods of SMT Heraeus, belong to binding material technical field.The present invention is using silicon powder as filler, prepare SMT Heraeus, silicon powder is not easy and other substance reactions, with most of acid, alkali not chemically reactive, its particle uniform fold is in object surface, it can make tension, the compression strength enhancing of solidfied material with stronger resistance to corrosion, wear-resisting property improves, and SILICA FUME purity is high, impurity content is low, and performance is stablized, and can reduce the exothermic peak temperature of epoxy resin cure reaction, the linear expansion coefficient and shrinking percentage for reducing solidfied material increase flame retardant property, to improve the high temperature resistance of SMT gluing sheet.The present invention passes through addition talcum powder, prepare SMT Heraeus, since talcum powder can be chemically reacted with the silicone functionalities in silane coupling agent, form the silicon oxygen bond with certain bonding force and protection, the thermic load for keeping coating on-going commitment certain, and high temperature adhesive force is increased, to improve the high temperature resistance of SMT Heraeus.
Description
Technical field
The present invention relates to a kind of preparation methods of SMT Heraeus, belong to binding material technical field.
Background technique
SMT is surface installation technique, is a kind of most popular technology and technique in current electronic assembly industry.SMT includes
Two kinds of entirely different techniques, it is a kind of to use solder(ing) paste；Another kind uses glue, is normally defined Heraeus, SMT Heraeus is
Applied to the special adhesive of surface-assembled, also known as surface-assembled adhesive, Heraeus.Former technique is to pass through halftone
Solder(ing) paste is coated on PCB, after surface mount device (being abbreviated as SMD) is installed, completes to connect with Reflow Soldering.Second
Technique is generally used for existing SMD, and has on the mixed type PCB of connector.Connector is connect by wave-soldering with PCB, in wave crest
Scolding tin is heated in weldering to fill out between component pin and insert hole to be connected and fixed.SMD can also use identical solder wave process, but member
Part must adhere to pcb board bottom, and piece is fallen when preventing wave-soldering, this bonding process is committed step.
Heraeus is that binder can be completed with the following method on pcb board for SMD to be bonded on PCB
Coating: scraper-type printing, the syringe-type dispensing for moving pin type print and using earliest, syringe-type dispensing include air pressure/time control
Or volume type control.After SMD is installed, binder must have enough wet strengths, by element it is fixed in position until
Solidification.Binder after solidification must have enough binding abilities that SMD and PCB connect together during wave-soldering, and
The electric property of element is not influenced after the completion of welding.Because glue must satisfy following demand: longer shelf life；Glue point is big
Small, shape keeps stable and consistent；Glue point shape is high, without hangover；Wet strength is high；Rapid curing；Nothing is collapsed in heat curing process
It falls into；High intensity is in conjunction with flexibility, heat shock resistance；Good electric property after solidification.
Patch red glue currently on the market is primarily present: glue point shape is bad；Wet strength is low；Solidification temperature is high, and speed is slow；
Cure shrinkage is big, and high temperature resistance is poor, it is high to fall part rate, therefore the use for being unable to satisfy the present and following high-end technique at all is wanted
It asks.
Since the size of present electronic component becomes smaller and smaller, for be easy to appear in encapsulation process part rate and
More stringent requirements are proposed for hot candied problem, and a kind of novel SMT Heraeus is researched and developed in design, and reaching expected properties of product seems especially
It is important.
Summary of the invention
The technical problems to be solved by the invention: it is poor for patch red glue high temperature resistance currently on the market, fall part rate
High problem provides a kind of preparation method of SMT Heraeus.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) by two amido diphenyl-methanes and bisphenol A type epoxy resin be added stirring at normal temperature in double-planet power mixer mix 10 ~
15min, then be placed in three-roll grinder and grind 1 ~ 3 time, obtain paste；
(2) bisphenol f type epoxy resin, epoxy-phenyl glycidol ether, rilanit special are added in double-planet power mixer
30 ~ 45min is stirred at 80 ~ 85 DEG C, must be mixed；
(3) it is passed through deionized water into stirred tank collet, mixture is made to be cooled to 30 ~ 35 DEG C, by paste, 2- ethyl -4- first
Base imidazoles, nano silica, talcum powder, silicon powder, vinyltriethoxysilane, carbon black are added into mixture, 30 ~
35 DEG C of 10 ~ 15min of stirred in water bath, obtain mixture；
(4) vacuum system is opened, mixture is placed in 1 ~ 1.5h of stirring under vacuum condition, then be placed in extruding and discharging in swager,
Obtain SMT Heraeus.
The bisphenol f type epoxy resin, bisphenol A type epoxy resin, phenyl glycidyl ether, two amido diphenyl-methanes,
2-ethyl-4-methylimidazole, rilanit special, nano silica, talcum powder, silicon powder, vinyltriethoxysilane, charcoal
Black parts by weight are 40 ~ 50 parts of bisphenol f type epoxy resins, 15 ~ 20 parts of bisphenol A type epoxy resins, 5 ~ 10 parts of phenyl glycidyls
Ether, 5 ~ 10 part of two amido diphenyl-methane, 1 ~ 5 part of 2-ethyl-4-methylimidazole, 1 ~ 3 part of rilanit special, 1 ~ 3 part of nano-silica
SiClx, 10 ~ 15 parts of talcum powder, 10 ~ 15 parts of silicon powders, 5 ~ 10 parts of vinyltriethoxysilane, 0.5 ~ 1 part of carbon black.
The specific preparation step of nano silica described in step (3) are as follows:
(1) sodium metasilicate is added in deionized water, 10 ~ 15min is stirred with 150 ~ 200r/min revolving speed under room temperature, it is molten to obtain sodium metasilicate
Liquid；
(2) cetyl trimethylammonium bromide is added in sodium silicate solution, 30 ~ 40 min of ultrasonic disperse, then is placed in 85 ~ 95 DEG C
20 ~ 30min is stirred with 150 ~ 200r/min revolving speed under water-bath, obtains sodium metasilicate mixed liquor；
(3) dehydrated alcohol is added in sodium metasilicate mixed liquor, is quickly stirred under 85 ~ 95 DEG C of water-baths with 500 ~ 600r/min revolving speed
40 ~ 60min adjusts pH to 6 ~ 7, obtains silicic acid gel；
(4) silicic acid gel is placed in air dry oven, the thermal dehydration 20 ~ for 24 hours at 110 ~ 120 DEG C obtains dewatered silicic acid
Gel；
(5) dewatered silicic acid gel is placed in baking oven, dry 1 ~ 2h, is ground into carefully with agate mortar at 120 ~ 140 DEG C
Powder, then be placed in Muffle furnace with 550 ~ 600 DEG C of 3 ~ 5h of temperature calcination, obtain nano silica.
The sodium metasilicate, cetyl trimethylammonium bromide, dehydrated alcohol, deionized water parts by weight be 25 ~ 30 parts
Sodium metasilicate, 0.1 ~ 0.3 part of cetyl trimethylammonium bromide, 10 ~ 15 parts of dehydrated alcohols, 40 ~ 50 parts of deionized waters.
PH described in step (3) adjusts the phosphoric acid using mass concentration 1%.
The average grain diameter of nano silica described in step (5) is 20 ~ 30nm.
The specific preparation step of silicon powder described in step (3) are as follows:
The quartz sand of 45 ~ 55 μm of grains of average grain diameter is placed in closed ball milling tank, at normal temperature with 150 ~ 200r/min revolving speed ball
8 ~ 10h is ground, then is placed at 110 ~ 120 DEG C and dries, obtains silicon powder.
The average grain diameter of the silicon powder is 0.1 ~ 0.3 μm.
The specification of talcum powder described in step (3) is 500 ~ 600 mesh, specific gravity is 2.6 ~ 2.8, and the average grain diameter of carbon black is 20
~ 60nm, specific gravity are 1.8 ~ 2.0.
Vacuum condition described in step (4) is 0.03 ~ 0.05MPa.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention prepares SMT Heraeus using silicon powder as filler, and silicon powder is a kind of nontoxic, tasteless, free of contamination inorganic
Nonmetallic materials, it has, and temperature tolerance is good, acid-alkali-corrosive-resisting, thermal coefficient are high, high insulation, low bulk, stable chemical performance, firmly
The excellent performances such as degree is big, silicon powder be not easy with other substance reactions, and most of acid, chemically reactive, particle be not equal for alkali
It is even to be covered on object surface, there is stronger resistance to corrosion, grain composition is reasonable, and when use can be reduced and eliminate precipitating, divides
Layer phenomenon can make tension, the compression strength enhancing of solidfied material, and wear-resisting property improves, and silicon powder purity is high, and impurity content is low,
Performance is stablized, and electrical insulation capability is excellent, so that solidfied material is had good insulation performance and arc resistance, can reduce epoxy resin
The exothermic peak temperature of curing reaction, reduces the linear expansion coefficient and shrinking percentage of solidfied material, and can increase the thermally conductive system of solidfied material
Number increases flame retardant property, to improve the high temperature resistance of SMT gluing sheet；
(2) present invention is by addition talcum powder, prepares SMT Heraeus, and talcum has lubricity, anti-stick, help stream, is fire resistance, anti-
Acidity, insulating properties, fusing point be high, chemically the excellent physics such as torpescence, covering power good, softness, good luster, strong adsorption force,
Chemical characteristic, since the crystal structure of talcum is in stratiform, so having the trend for easily splitting into scale and special lubricious
Property, talcum powder can be chemically reacted with the silicone functionalities in vinyltriethoxysilane, be formed with certain bonding
The silicon oxygen bond of power and protection, the thermic load for keeping coating on-going commitment certain, and high temperature adhesive force is increased, to improve
The high temperature resistance of SMT Heraeus；
(3) present invention prepares SMT Heraeus, nano silica is a kind of inorganic chemical industry material by addition nano silica
Material, is ultrafine nanometer inorganic material, have anti-ultraviolet optical property can be improved SMT Heraeus anti-aging property,
Mechanical strength and chemical-resistance, nanometer grade silica are amorphous white powder, nontoxic, tasteless, pollution-free, and micro-structure is
Spherical shape, in cotton-shaped and netted quasi- grain structure, the addition of nano Si 02 can be in the coated one layer of organic material of epoxy resin surface
Material forms network structure, forms a kind of masonry structure, and epoxy resin is made to have certain hydrophobicity, can inhibit colloid flowing, adds
Fast curing rate improves bond effect, can effectively increase the leakproofness and barrier properties of SMT Heraeus, will be through surface-active-treatment
Nano silica afterwards is well dispersed in modifying epoxy resin by organosilicon encapsulation gel matrix, can significantly shorten encapsulation
The material solidification time, and solidification temperature can be reduced to room temperature, and the sealing performance of SMT Heraeus is made to be significantly improved, and increase SMT
Nanometer silicon dioxide particle is sufficiently and uniformly distributed in epoxide resin material, can improve comprehensively by the service life of Heraeus
Epoxy-based material performance, improves its mechanical strength and elongation percentage, improves wearability, and improve SMT ageing-resistant performance and
Heat-resisting quantity.
Specific embodiment
The quartz sand of 45 ~ 55 μm of grains of average grain diameter is placed in closed ball milling tank, is turned at normal temperature with 150 ~ 200r/min
Fast 8 ~ 10h of ball milling, then be placed at 110 ~ 120 DEG C and dry, 0.1 ~ 0.3 μm of average grain diameter of silicon powder is obtained, according to parts by weight, point
Also known as measure 25 ~ 30 parts of sodium metasilicate, 0.1 ~ 0.3 part of cetyl trimethylammonium bromide, 10 ~ 15 parts of dehydrated alcohols, 40 ~ 50 parts go from
Sodium metasilicate is added in deionized water sub- water, stirs 10 ~ 15min under room temperature with 150 ~ 200r/min revolving speed, it is molten to obtain sodium metasilicate
Cetyl trimethylammonium bromide is added in sodium silicate solution, 30 ~ 40 min of ultrasonic disperse, then is placed in 85 ~ 95 DEG C of water-baths by liquid
Under with 150 ~ 200r/min revolving speed stir 20 ~ 30min, obtain sodium metasilicate mixed liquor, by dehydrated alcohol be added sodium metasilicate mixed liquor in,
40 ~ 60min is stirred quickly with 500 ~ 600r/min revolving speed under 85 ~ 95 DEG C of water-baths, with the phosphorus acid for adjusting pH of mass concentration 1% to 6
~ 7, silicic acid gel is obtained, silicic acid gel is placed in air dry oven, the thermal dehydration 20 ~ for 24 hours at 110 ~ 120 DEG C, after obtaining dehydration
Silicic acid gel, dewatered silicic acid gel is placed in baking oven, dry 1 ~ 2h, is ground with agate mortar at 120 ~ 140 DEG C
It at fine powder, then is placed in Muffle furnace with 550 ~ 600 DEG C of 3 ~ 5h of temperature calcination, obtains the nano silica of 20 ~ 30nm of partial size, then
According to parts by weight, 40 ~ 50 parts of bisphenol f type epoxy resins, 15 ~ 20 parts of bisphenol A type epoxy resins, the contracting of 5 ~ 10 phenyl are weighed respectively
Water glycerin ether, 5 ~ 10 part of two amido diphenyl-methane, 1 ~ 5 part of 2-ethyl-4-methylimidazole, 1 ~ 3 part of rilanit special, 1 ~ 3 part receive
Rice silica, 10 ~ 15 parts of talcum powder, 10 ~ 15 parts of silicon powders, 5 ~ 10 parts of vinyltriethoxysilane, 0.5 ~ 1 part of carbon black,
Stirring at normal temperature in double-planet power mixer is added in two amido diphenyl-methanes and bisphenol A type epoxy resin and mixes 10 ~ 15min,
It is placed in three-roll grinder and grinds 1 ~ 3 time again, obtain paste, by bisphenol f type epoxy resin, epoxy-phenyl glycidol ether, hydrogen
Change castor oil and 30 ~ 45min of stirring at 80 ~ 85 DEG C is added in double-planet power mixer, mixture is obtained, into stirred tank collet
It is passed through deionized water, mixture is made to be cooled to 30 ~ 35 DEG C, by paste, 2-ethyl-4-methylimidazole, nano silica, cunning
Mountain flour, silicon powder, vinyltriethoxysilane, carbon black are added into mixture, 30 ~ 35 DEG C of stirred in water bath 10 ~
15min obtains mixture, opens vacuum system, mixture is placed in 1 ~ 1.5h of stirring under vacuum condition, then be placed in swager and squeeze
Material is extruded, SMT Heraeus is obtained.
The quartz sand of 45 μm of grains of average grain diameter is placed in closed ball milling tank, at normal temperature with 150r/min revolving speed ball milling
8h, then be placed at 110 DEG C and dry, obtains 0.1 μm of average grain diameter of silicon powder, according to parts by weight, weigh respectively 25 parts of sodium metasilicate,
0.1 part of cetyl trimethylammonium bromide, 10 parts of dehydrated alcohols, 40 parts of deionized waters sodium metasilicate are added in deionized water, often
10min is stirred with 150r/min revolving speed under temperature, sodium silicate solution is obtained, sodium silicate solution is added in cetyl trimethylammonium bromide
In, ultrasonic disperse 30min, then be placed under 85 DEG C of water-baths and 20min is stirred with 150r/min revolving speed, sodium metasilicate mixed liquor is obtained, by nothing
Water-ethanol is added in sodium metasilicate mixed liquor, 40min is quickly stirred under 85 DEG C of water-baths with 500r/min revolving speed, with mass concentration 1%
Phosphorus acid for adjusting pH to 6, obtain silicic acid gel, silicic acid gel be placed in air dry oven, thermal dehydration 20h, obtains at 110 DEG C
Dewatered silicic acid gel is placed in baking oven by dewatered silicic acid gel, and dry 1h, is ground with agate mortar at 120 DEG C
It at fine powder, then is placed in Muffle furnace with 550 DEG C of temperature calcination 3h, obtains the nano silica of partial size 20nm, then by weight
Number meter, weighs 40 parts of bisphenol f type epoxy resins, 15 parts of bisphenol A type epoxy resins, 5 phenyl glycidyl ethers, 5 parts of diamines respectively
Base diphenyl-methane, 1 part of 2-ethyl-4-methylimidazole, 1 part of rilanit special, 1 part of nano silica, 10 parts of talcum powder, 10 parts
Two amido diphenyl-methanes and bisphenol A type epoxy resin are added for silicon powder, 5 parts of vinyltriethoxysilane, 0.5 part of carbon black
Stirring at normal temperature mixes 10min in double-planet power mixer, then is placed in three-roll grinder and grinds 1 time, paste is obtained, by bis-phenol
F type epoxy resin, epoxy-phenyl glycidol ether, rilanit special are added in double-planet power mixer and stir at 80 DEG C
30min obtains mixture, is passed through deionized water into stirred tank collet, and mixture is made to be cooled to 30 DEG C, by paste, 2- ethyl-
4-methylimidazole, nano silica, talcum powder, silicon powder, vinyltriethoxysilane, carbon black are added into mixture,
In 30 DEG C of stirred in water bath 10min, mixture is obtained, vacuum system is opened, mixture is placed under vacuum condition and stirs 1h, then is set
The extruding and discharging in swager obtains SMT Heraeus.
The quartz sand of 50 μm of grains of average grain diameter is placed in closed ball milling tank, at normal temperature with 175r/min revolving speed ball milling
9h, then be placed at 115 DEG C and dry, obtains 0.2 μm of average grain diameter of silicon powder, according to parts by weight, weigh respectively 27 parts of sodium metasilicate,
0.2 part of cetyl trimethylammonium bromide, 13 parts of dehydrated alcohols, 45 parts of deionized waters sodium metasilicate are added in deionized water, often
13min is stirred with 175r/min revolving speed under temperature, sodium silicate solution is obtained, sodium silicate solution is added in cetyl trimethylammonium bromide
In, ultrasonic disperse 35min, then be placed under 90 DEG C of water-baths and 25min is stirred with 175r/min revolving speed, sodium metasilicate mixed liquor is obtained, by nothing
Water-ethanol is added in sodium metasilicate mixed liquor, 50min is quickly stirred under 90 DEG C of water-baths with 550r/min revolving speed, with mass concentration 1%
Phosphorus acid for adjusting pH to 6.5, obtain silicic acid gel, silicic acid gel be placed in air dry oven, the thermal dehydration 22h at 115 DEG C,
Dewatered silicic acid gel is obtained, dewatered silicic acid gel is placed in baking oven, dry 1.5h, uses agate mortar at 130 DEG C
It is ground into fine powder, then is placed in Muffle furnace with 575 DEG C of temperature calcination 4h, obtains the nano silica of partial size 25nm, then by weight
Number meter is measured, weighs 45 parts of bisphenol f type epoxy resins, 17 parts of bisphenol A type epoxy resins, 7 phenyl glycidyl ethers, 7 parts respectively
Two amido diphenyl-methanes, 3 parts of 2-ethyl-4-methylimidazoles, 2 parts of rilanit specials, 2 parts of nano silicas, 13 parts of talcum powder,
13 parts of silicon powders, 7 parts of vinyltriethoxysilane, 0.7 part of carbon black, by two amido diphenyl-methanes and bisphenol A type epoxy resin
Stirring at normal temperature in double-planet power mixer is added and mixes 13min, then is placed in three-roll grinder and grinds 2 times, obtains paste, it will
Bisphenol f type epoxy resin, epoxy-phenyl glycidol ether, rilanit special are added in double-planet power mixer and stir at 83 DEG C
37min is mixed, mixture is obtained, is passed through deionized water into stirred tank collet, mixture is made to be cooled to 33 DEG C, by paste, 2- second
Base -4-methylimidazole, nano silica, talcum powder, silicon powder, vinyltriethoxysilane, carbon black are added to mixture
In, in 33 DEG C of stirred in water bath 13min, mixture is obtained, vacuum system is opened, mixture is placed under vacuum condition and is stirred
1.3h, then it is placed in extruding and discharging in swager, obtain SMT Heraeus.
The quartz sand of 55 μm of grains of average grain diameter is placed in closed ball milling tank, at normal temperature with 200r/min revolving speed ball milling
10h, then be placed at 120 DEG C and dry, 0.3 μm of average grain diameter of silicon powder is obtained, according to parts by weight, weighs 30 parts of silicic acid respectively
Sodium, 0.3 part of cetyl trimethylammonium bromide, 15 parts of dehydrated alcohols, 50 parts of deionized waters, are added deionized water for sodium metasilicate
In, 15min is stirred with 200r/min revolving speed under room temperature, sodium silicate solution is obtained, silicic acid is added in cetyl trimethylammonium bromide
In sodium solution, 40 min of ultrasonic disperse, then be placed under 95 DEG C of water-baths and 230min is stirred with 200r/min revolving speed, obtain sodium metasilicate mixing
Dehydrated alcohol is added in sodium metasilicate mixed liquor, quickly stirs 60min under 95 DEG C of water-baths with 600r/min revolving speed, use matter by liquid
The phosphorus acid for adjusting pH of concentration 1% is measured to 7, silicic acid gel is obtained, silicic acid gel is placed in air dry oven, heated at 120 DEG C de-
Water for 24 hours, obtains dewatered silicic acid gel, and dewatered silicic acid gel is placed in baking oven, and dry 2h, uses agate at 140 DEG C
Mortar grinder is at fine powder, then is placed in Muffle furnace with 600 DEG C of temperature calcination 5h, obtains the nano silica of partial size 30nm, then
According to parts by weight, 50 parts of bisphenol f type epoxy resins, 20 parts of bisphenol A type epoxy resins, 10 phenyl glycidyls are weighed respectively
Ether, 10 part of two amido diphenyl-methane, 5 parts of 2-ethyl-4-methylimidazoles, 3 parts of rilanit specials, 3 parts of nano silicas, 15 parts
Talcum powder, 15 parts of silicon powders, 10 parts of vinyltriethoxysilane, 1 part of carbon black, by two amido diphenyl-methanes and bisphenol-A type ring
Oxygen resin is added stirring at normal temperature in double-planet power mixer and mixes 15min, then is placed in three-roll grinder and grinds 3 times, obtains cream
Bisphenol f type epoxy resin, epoxy-phenyl glycidol ether, rilanit special are added in double-planet power mixer shape object
45min is stirred at 85 DEG C, obtains mixture, is passed through deionized water into stirred tank collet, mixture is made to be cooled to 35 DEG C, by paste
Object, 2-ethyl-4-methylimidazole, nano silica, talcum powder, silicon powder, vinyltriethoxysilane, carbon black be added to
In mixture, in 35 DEG C of stirred in water bath 15min, mixture is obtained, vacuum system is opened, mixture is placed under vacuum condition and is stirred
1.5h is mixed, then is placed in extruding and discharging in swager, obtains SMT Heraeus.
The Heraeus that SMT Heraeus prepared by the present invention and Fujian company produce is detected, specific testing result
Such as the following table 1:
Detection method:
The SMT Heraeus that above embodiments are prepared and the Heraeus of Fujian company production are according to standard SJ/T11187-
1998, which test, is tested for the property.
Table 1SMT Heraeus performance characterization
SMT Heraeus prepared by the present invention as shown in Table 1, solidification temperature is low, and curing time is short, solidifies the hard bubble-free of rear surface
It generates, excellent combination property can be widely applied in various components, have a vast market value and application prospect.
Claims (10)
1. a kind of preparation method of SMT Heraeus, which is characterized in that specific preparation step are as follows:
(1) by two amido diphenyl-methanes and bisphenol A type epoxy resin be added stirring at normal temperature in double-planet power mixer mix 10 ~
15min, then be placed in three-roll grinder and grind 1 ~ 3 time, obtain paste；
(2) bisphenol f type epoxy resin, epoxy-phenyl glycidol ether, rilanit special are added in double-planet power mixer
30 ~ 45min is stirred at 80 ~ 85 DEG C, must be mixed；
(3) it is passed through deionized water into stirred tank collet, mixture is made to be cooled to 30 ~ 35 DEG C, by paste, 2- ethyl -4- first
Base imidazoles, nano silica, talcum powder, silicon powder, vinyltriethoxysilane, carbon black are added into mixture, 30 ~
35 DEG C of 10 ~ 15min of stirred in water bath, obtain mixture；
(4) vacuum system is opened, mixture is placed in 1 ~ 1.5h of stirring under vacuum condition, then be placed in extruding and discharging in swager,
Obtain SMT Heraeus.
2. a kind of preparation method of SMT Heraeus according to claim 1, which is characterized in that the bisphenol F type epoxy
Resin, bisphenol A type epoxy resin, phenyl glycidyl ether, two amido diphenyl-methanes, 2-ethyl-4-methylimidazole, hydrogenated castor
Oil, nano silica, talcum powder, silicon powder, vinyltriethoxysilane, the parts by weight of carbon black are 40 ~ 50 parts of bisphenol-f type
Epoxy resin, 15 ~ 20 parts of bisphenol A type epoxy resins, 5 ~ 10 parts of phenyl glycidyl ethers, 5 ~ 10 part of two amido diphenyl-methane, 1 ~ 5
Part 2-ethyl-4-methylimidazole, 1 ~ 3 part of rilanit special, 1 ~ 3 part of nano silica, 10 ~ 15 parts of talcum powder, 10 ~ 15 parts of silicon
Micro mist, 5 ~ 10 parts of vinyltriethoxysilane, 0.5 ~ 1 part of carbon black.
3. a kind of preparation method of SMT Heraeus according to claim 1, which is characterized in that nanometer described in step (3)
The specific preparation step of silica are as follows:
(1) sodium metasilicate is added in deionized water, 10 ~ 15min is stirred with 150 ~ 200r/min revolving speed under room temperature, it is molten to obtain sodium metasilicate
Liquid；
(2) cetyl trimethylammonium bromide is added in sodium silicate solution, 30 ~ 40 min of ultrasonic disperse, then is placed in 85 ~ 95 DEG C
20 ~ 30min is stirred with 150 ~ 200r/min revolving speed under water-bath, obtains sodium metasilicate mixed liquor；
(3) dehydrated alcohol is added in sodium metasilicate mixed liquor, is quickly stirred under 85 ~ 95 DEG C of water-baths with 500 ~ 600r/min revolving speed
40 ~ 60min adjusts pH to 6 ~ 7, obtains silicic acid gel；
(4) silicic acid gel is placed in air dry oven, the thermal dehydration 20 ~ for 24 hours at 110 ~ 120 DEG C obtains dewatered silicic acid
Gel；
(5) dewatered silicic acid gel is placed in baking oven, dry 1 ~ 2h, is ground into carefully with agate mortar at 120 ~ 140 DEG C
Powder, then be placed in Muffle furnace with 550 ~ 600 DEG C of 3 ~ 5h of temperature calcination, obtain nano silica.
4. a kind of preparation method of SMT Heraeus according to claim 3, which is characterized in that the sodium metasilicate, 16
Alkyl trimethyl ammonium bromide, dehydrated alcohol, deionized water parts by weight be 25 ~ 30 parts of sodium metasilicate, 0.1 ~ 0.3 part of cetyl three
Methyl bromide ammonium, 10 ~ 15 parts of dehydrated alcohols, 40 ~ 50 parts of deionized waters.
5. a kind of preparation method of SMT Heraeus according to claim 3, which is characterized in that pH tune described in step (3)
Save the phosphoric acid using mass concentration 1%.
6. a kind of preparation method of SMT Heraeus according to claim 3, which is characterized in that nanometer described in step (5)
The average grain diameter of silica is 20 ~ 30nm.
7. a kind of preparation method of SMT Heraeus according to claim 1, which is characterized in that silicon described in step (3) is micro-
The specific preparation step of powder are as follows:
The quartz sand of 45 ~ 55 μm of grains of average grain diameter is placed in closed ball milling tank, at normal temperature with 150 ~ 200r/min revolving speed ball
8 ~ 10h is ground, then is placed at 110 ~ 120 DEG C and dries, obtains silicon powder.
8. a kind of preparation method of SMT Heraeus according to claim 7, which is characterized in that the silicon powder is put down
Equal partial size is 0.1 ~ 0.3 μm.
9. a kind of preparation method of SMT Heraeus according to claim 1, which is characterized in that talcum described in step (3)
The specification of powder is 500 ~ 600 mesh, specific gravity is 2.6 ~ 2.8, and the average grain diameter of carbon black is 20 ~ 60nm, specific gravity is 1.8 ~ 2.0.
10. a kind of preparation method of SMT Heraeus according to claim 1, which is characterized in that true described in step (4)
Empty condition is 0.03 ~ 0.05MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111892058A (en) * | 2020-07-04 | 2020-11-06 | 江苏联瑞新材料股份有限公司 | Superfine silicon powder for surface mount discrete device and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020127406A1 (en) * | 2001-01-11 | 2002-09-12 | International Business Machines Corporation | Epoxy-siloxanes based electrically conductive adhesives for semiconductor assembly and process for use thereof |
| CN1872936A (en) * | 2005-05-31 | 2006-12-06 | 北京联合钛得胶粘剂有限公司 | Rapid solidifed mesothermal epoxy patch glue in monocomponent, and preparation method |
| CN105315941A (en) * | 2015-11-23 | 2016-02-10 | 苏州盖德精细材料有限公司 | Heatproof and fireproof SMT adhesive and preparing method thereof |
-
2019
- 2019-02-25 CN CN201910137073.8A patent/CN110003833A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020127406A1 (en) * | 2001-01-11 | 2002-09-12 | International Business Machines Corporation | Epoxy-siloxanes based electrically conductive adhesives for semiconductor assembly and process for use thereof |
| CN1872936A (en) * | 2005-05-31 | 2006-12-06 | 北京联合钛得胶粘剂有限公司 | Rapid solidifed mesothermal epoxy patch glue in monocomponent, and preparation method |
| CN105315941A (en) * | 2015-11-23 | 2016-02-10 | 苏州盖德精细材料有限公司 | Heatproof and fireproof SMT adhesive and preparing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111892058A (en) * | 2020-07-04 | 2020-11-06 | 江苏联瑞新材料股份有限公司 | Superfine silicon powder for surface mount discrete device and preparation method thereof |
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