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CN102276988B - Mono-component Ni-C filled-type FIP (Form In Place) heat-curing highly-conductive silicone rubber and preparation method thereof - Google Patents

Mono-component Ni-C filled-type FIP (Form In Place) heat-curing highly-conductive silicone rubber and preparation method thereof Download PDF

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CN102276988B
CN102276988B CN2011101520743A CN201110152074A CN102276988B CN 102276988 B CN102276988 B CN 102276988B CN 2011101520743 A CN2011101520743 A CN 2011101520743A CN 201110152074 A CN201110152074 A CN 201110152074A CN 102276988 B CN102276988 B CN 102276988B
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ethenyl blocking
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CN102276988A (en
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夏志东
周虎
刘小黑
李莹
郭福
史耀武
雷永平
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Beijing University of Technology
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Abstract

The invention discloses mono-component Ni-C filled-type FIP (Form In Place) heat-curing highly-conductive silicone rubber and a preparation method thereof, belonging to the technical field of rubber materials. The rubber comprises the following components in parts by weight: 52.5-62.5 parts of vinyl-terminated polydimethyl siloxane containing white carbon black (1), 37.5-47.5 parts of low-viscosity vinyl-terminated polydimethyl siloxane (2), 195-210 parts of Ni-C conductive filling material (3), 0.1-0.15 part of alcohol inhibitor (4), 2.8-3.2 parts of Si-H based line-shaped methyl hydrogen polysiloxane cross-linking agent (5), 0.1-0.2 part of Kaarst platinum accelerating agent and 0.05-1 part of thixotropic agent (7). The preparation method comprises the following steps of: uniformly mixing the component (1) with the component (2); sequentially adding the component (3), the component (4), the component (5), the component (6) and the component (7); and uniformly mixing at a certain temperature, vacuum degree and stirring speed, wherein each time interval is 20-60min. The rubber can be applied to on-site forming and a shielding shell with a tiny size and compact structure.

Description

A kind of single-component Ni-C filled FIP hot sulfurization high-conductivity silicon rubber and preparation method thereof
Technical field
The invention belongs to the elastomeric material technical field, relate to a kind of single-component Ni-C filled hot sulfurization high-conductivity silicon rubber mixture, be specifically related to conductive silicon rubber by nickel coated graphite powder and nickel bag filled with carbon fibers.
Background technology
In recent years, along with the high speed development of electronic technology, the surge of various wireless communication systems and high-frequency electron device quantity causes new environmental pollution---and Electromagnetic Interference (Electromagnetic interference, EMI).The EMI that electromagnetic radiation produces not only has influence on the realization of electronic product performance, and the electromagnetic pollution that causes therefrom also can cause serious harm with other organism to human.For solving interference and the leakage that electromagnetic radiation causes, mainly adopt electromagnetic shielding material to shield, the electromagnetic compatible environment that the realization electronic and electrical equipment is in harmonious proportion, coexists mutually with environmental facies (Electromagnetic compatibility, EMC).
The conventional conductive rubber of punching and shaping, die forming or extrusion molding; After the shape and size that are processed into design, through fluting installation, bonding or bolt location, directly as the conductive elastomer liner; Can be applicable in the cabinet or shell of large-size electronic installation; Make case shell seam crossing conduction continuously,, make it to satisfy the electromagnetic compatibility requirement so that enough shielding propertiess to be provided.
Miniaturized along with electronics; Like mobile phone, palm PC (Personal Digital Assistant; PDA), (conventional conductive rubber receives actual production technique and limits with manufacturing cost PC for Personal Computer, PC) card etc.; Can't satisfy the request for utilization in, the complex structure shield shell small at volume, some glue shaping conductive rubber is complied with the demand of this technical development and is arisen at the historic moment.
Point glue is shaped, be otherwise known as on-the-spotly be shaped, be shaped on the spot, original position is shaped, glue is dripped on surface point glue and surface, the manufacturing process that refers to conductive rubber is translated from English Form-In-Place (FIP).The FIP conductive rubber requires rubber to have good flowing property and thixotropy, and the viscosity of basic glue is at 10-60PaS, with the adhesive tape of extruding after conductive filler material mixes can the original position shaping.The size of FIP adhesive tape and extrusion capacity all with the viscosity of conductive rubber, the size of used pressure and used Glue dripping head internal diameter is relevant when extruding.Need consider the size of filled conductive filler and the viscosity and the thixotropic property of conductive rubber for undersized adhesive tape, in order to obtain the conductive rubber of suitable on-the-spot some glue, the amount of the metal powder of filling is difficult for excessive.Liquid silastic has good flowability, and its viscosity does not wait from 3-100PaS, the condition of compound preparation FIP conductive rubber, and be high-elastic gonosome after the sulfuration, can play the effect of sealing during pressurized through its distortion.FIP conductive rubber sulfuration back is not very high with the bonding strength of substrate or workpiece, makes things convenient for the maintenance and the maintenance of equipment.HV macromolecular material flowability is not the fine scene point glue that is not suitable for carrying out, and thermoplasticity and thermosetting resin sulfuration back hardness is very big, the very little effect that can not play sealing of compression set, and bonding strength is big, not easy-clear.
FIP conductive rubber and conventional conductive rubber phase are than having a lot of advantages: (1) can reduce materials consumption and practice thrift cost.Traditional process method is to process the conductive rubber lining with die-cut mode, therefore can produce a lot of scrap stock, and these waste materials can't utilize again, and what how many FIP conductive rubbers can put according to specified size with, do not produce waste material.(2) the simplification production technique is raised the efficiency, satisfied harsh assembly space limits has wider range of application.Especially the FIP conductive rubber of single-component can directly use and need not mix, and formation liner and substrate form permanent bonding under heating, and working method is simple.Traditional conductive rubber also need assemble groove and the positioning screw hole that matches with washer-shaped, has increased time of setting-up and manufacturing cost.And through regulating Glue dripping head internal diameter size and putting the adhesive tape that glue pressure size can reach different size, the smallest cross-sectional size of some glue liner can reach 0.6mm (wide) * 0.4mm (height), can satisfy harsh assembly space.(3) has the robotization FIP spot gluing equipment of easy control simple to operate.In industrial application; The spot gluing equipment spot printing FIP conductive rubber that uses a computer and control; Need not costly precision die; Get final product accurate and exactly that shape is consistent colloid point and be applied to original position shaping on the specified small flange surface, satisfied the demand that reaches rapid growth in enormous quantities in the automatic production greatly.Because these characteristics and advantage, FIP conductive rubber technology becomes the minimum shielding scheme of total cost, is being applied to more and more in the electronics of complex structure, packing compactness.
Patent CN101624471A (March 6 2009 applying date; Open day on January 13rd, 2010) having announced a kind of is that the mode of 10-150 μ m conductive particle has prepared the in-place forming conductive silicon rubber through in the ethenyl blocking YSR 3286, adding 100-500 weight part particle size, but when metal-powder when certain part by weight (threshold value) is following, conductive path cannot form; Electroconductibility is very poor; And the metal-powder of filling has not only increased material cost when too many, and too much filler particles also can make the mobile of glue significantly descend; Thereby influence on-the-spot gluing process, mechanical property also can descend to some extent simultaneously.In the ethenyl blocking YSR 3286 of 50000mPa.s viscosity, volume specific resistance just is 0.008 Ω cm when silver-coated copper powder end addition reaches 400 weight parts like patent CN101624471A instance 1.In addition, this patent sulfidization molding temperature is 150 ℃, the device of on-the-spot some glue easy temperature influence when sulfuration.
U.S. Pat 5910524 (the applying date: on October 6th, 1997; Open day: announced a kind ofly prepared the in-place forming conducing composite material on June 8th, 1999) that its volume specific resistance is 500-1000m Ω cm through the mode of in containing the silicone resin of vinyl, adding auxiliary agents such as nickel coated graphite powder, hydrogenous siloxane crosslinker, platinum catalyst.Mentioning conducing composite material conductive particle loading level in the instance 1 is 56%, and its resistivity is 334-6356m Ω cm.Have this to find out, the filling umber of the conductive filler material of single variety is not enough, and the conductive path of formation is few, and electroconductibility is bad.In addition, the conducing composite material that is prepared by silicon resin base is a thermosetting material, is not suitable for resilient seal and uses.
U.S. Pat 7537712 (the applying date: on March 3rd, 2003; Open day: on May 26th, 2009) announced that a kind of conductive silicon rubber composition comprises that each molecule of (A) 100 weight parts has the organopolysiloxane of at least two alkenyls; (B) each molecule has the organopolysiloxane (consumption is enough to solidify compsn of the present invention) of at least two silicon bonded hydrogen atom; (C) platinum catalyst (consumption is enough to promote the curing of the present composition); (D) 50-5000 weight part metal-based conductive filler material and (E) 5-500 weight part surfactant content be not more than the spherical silicone rubber particles of weight percent 0.3%.Because the umber of filler (metal-based+rubber powder) is a lot, mobile poor, be not suitable for the on-the-spot gum forming of putting, in addition, sulfidization molding immediately after the mixing can not prolonged preservation.
In sum: conductive silicon oxyalkyl matrix material also exists following problem and difficulty not to overcome at present: (1) particles filled amount is big, causes flowability and even gluing process poor performance.The conductive filler material of single shape can not form effective conductive channel when the filling umber seldom, quantity conductivity very little is bad, improves loading level in order to improve conductivity, must sacrifice its flowability again, thereby can not on-the-spot some glue.(2) be that the matrix material of matrix is a plastic material with the heat-curable silicone, be not suitable for as elaxtic seal; (3) 150 ℃ curing temperature has reduced the range of application of conductive silicon rubber, requires workpiece or the device can anti-150 ℃ temperature and relevant use properties is constant.
Summary of the invention
The present invention provides a kind of single-component Ni-C filled FIP hot sulfurization high-conductivity silicon rubber matrix material and preparation method thereof in order to overcome above-mentioned difficulties and to satisfy above-mentioned requirements, is used for the elasticity electromagnetic sealing of electronic and electrical equipment.
The high conductive silicon compounded rubber of a kind of single-component Ni-C filled FIP hot sulfurization provided by the invention is characterized in that comprise following material: (1) 52.5-62.5 weight part contains the ethenyl blocking YSR 3286 of WHITE CARBON BLACK; (2) the LV ethenyl blocking YSR 3286 of 37.5-47.5 weight part; (3) the Ni-C conductive filler material of 195-210 weight part median size 7 μ m-200 μ m; (4) 0.1-0.15 weight part alkynol suppressor factor; (5) the linear methylhydrogenpolysi,oxane linking agent of 2.8-3.2 weight part Si-H base, hydrogen matrix amount per-cent 0.4-0.8%; (6) the Ka Ersite platinum catalyst of 0.1-0.2 weight part, Pt content 3000-5000ppm; (7) thixotropic agent of 0.05-1 weight part.
Described Ni-C conductive filler material is meant nickel coated graphite powder and nickel bag thomel.Be applied to require the electromagnetic shielding of in-place forming and the electronics of environmental sealing.
The ethenyl blocking YSR 3286 of WHITE CARBON BLACK in (1) wherein, the content of WHITE CARBON BLACK is 20%-40%, and the viscosity of ethenyl blocking YSR 3286 is 5000-20000mPas, and the vinyl mass percent is 0.26%-0.28%.
(2) LV ethenyl blocking YSR 3286 in, the LV ethenyl blocking YSR 3286 of one or more different viscosity, viscosity is 1000-2000mPas, contents of ethylene is 0.7%-0.8%.
(3) nickel coated graphite powder and the 28-30 part diameter of the preferred 167-180 part of Ni-C conductive filler material median size 50 μ m-100 μ m of nickel coated graphite powder and nickel bag thomel are 7-10 μ m in, and length is the nickel bag thomel of 100-200 μ m.
(4) the alkynol suppressor factor described in is the acetylene hexalin.
The preparation method of the high conductive silicon compounded rubber of above-mentioned a kind of single-component Ni-C filled FIP hot sulfurization may further comprise the steps:
(1) mix with LV ethenyl blocking YSR 3286 at 100 ℃ of ethenyl blocking YSR 3286s that will contain WHITE CARBON BLACK down, vacuumize assurance pressure reduction >=0.09MPa, continuously stirring 4-6 hour, stirring-head 4-10RPM disperseed a 57-114RPM.
(2) the Ni-C conductive filler material of adding nickel coated graphite powder and nickel bag thomel on the basis of (1): add nickel bag thomel earlier; Add remaining nickel coated graphite powder more in batches, mix after 20-30 minute at every turn and add next batch again, last continuously stirring 4-6 hour; 100 ℃ of temperature; Vacuumize assurance pressure reduction >=0.09MPa, stirring-head 4-10RPM disperses a 57-114RPM.
(3) on the basis of (2), add suppressor factor, add in batches, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour, 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM.
(4) on the basis of (3), add linking agent, add in batches, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour, 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM.
(5) on the basis of (4), add catalyzer, add in batches, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour, 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM.
(6) on the basis of (5), add thixotropic agent, disposable adding, stirred 0.5 hour last intermittence, and 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM.
Inventive principle:
Why rubber can conduct electricity is because added metallic particles or the composite particles with satisfactory electrical conductivity; Ni-C type conductive filler material is exactly on the carbon material of the relative metal difference of electroconductibility, to coat one deck nickel metal; Nickel coated graphite powder is to use more a kind of composite powder; Because the surface has coated one deck nickel, electroconductibility is greatly improved.The mechanism of general conductive rubber conduction has three kinds: contact with each other the conductive network of formation between (1) particle, i.e. conductive path; (2) when the distance of two conductive particles is very little because thermal vibration, thereby the conductive network that electronics can the migration between conducting particles forms; (3) if the conducting particles internal electric field is very strong, electronics has very big probability leap polymer interface potential barrier, transits on the adjacent charged, produces autoelectronic current.Form conductive network.When forming conductive network through first kind of mechanism; The electroconductibility of conductive rubber just can be fine; And the probability that the adding of nickel bag thomel can make particle be in contact with one another under the situation that contains the identical weight umber becomes big, thereby forms conductive path more easily, obtains the material that meets of good conductivity.Can obtain single-component Ni-C filled FIP hot sulfurization high-conductivity silicon rubber through the above-mentioned steps preparation.The interpolation that wherein must be noted that each component reaches relevant processing parameter in proper order; The viscosity influence of temperature convection body is very big; Zylox is typical non-Newtonian fluid; The temperature low more characteristic of HV is more arranged, therefore, make that the conductive filler material dispersive is more even 100 ℃ of viscosity that can effectively reduce Zylox down.Can remove the organic molecule that remains in the Zylox under this temperature simultaneously, these small molecules are that organic products produces in the preparation process.Residual small molecules can make conductive rubber when sulfuration, produce pore.The fusing point of acetylene hexalin is 30-33 ℃, when room temperature is lower, need mix down at 40 ℃, can prevent the crystallization of suppressor factor acetylene hexalin, avoids the suppressor factor skewness.Vacuum condition helps to be adsorbed on overflowing of gas on the conductive filler material, and these gases can make conductive rubber when sulfuration, produce pore.Thixotropic agent can form effective three-dimensional network through the hydrogen bonded between the polar molecule group; Under whipped state, hydrogen bond is destroyed, thereby viscosity diminishes; Hydrogen bond meeting recombine when stirring stops; Therefore improved the thixotropy of conductive rubber, the shape of conductive rubber does not change a lot behind the on-the-spot point of the assurance glue, but stirring can make the three-dimensional network of formation rupture and can not recover fully for a long time; Thereby reduced the effect of thixotropic agent, so the churning time of thixotropic agent when mixing can not surpass 30mins.Here the interpolation order of various auxiliary agents requires emphasis; Suppressor factor will add before linking agent and catalyzer; The situation that spot cure only after the suppressor factor thorough mixing is even, just can not occur; Because when not having suppressor factor, linking agent and catalyzer can impel the sulfuration of rubber at once.Certain negative pressure can make the boiling point lowering of material; When pressure was 1.27KPa, the boiling point of acetylene hexalin had only 66 ℃, so temperature will be at 40 ℃ in the mixing process; Temperature is too high can quicken the volatilization of suppressor factor, the low excessively suppressor factor crystalline situation that prevents that do not have of temperature.Need cryopreservation after this composite gum is mixed, treat during use to utilize the direct point of spot gluing equipment to be overlying on the workpiece after it gets back to room temperature.
This material has following characteristics: (1) uses nickel coated graphite powder+nickel bag thomel composite conducting particle to come filled silicon rubber, can the effective conductive path of performance, and reduce total filling umber of conductive filler material and satisfy the correlated performance requirement; (2) through preparation technology and additive, make glue have good flowability and thixotropic property, can satisfy the request for utilization that rapid processing and original position are shaped.(3) can be applicable on the electronic electric equipment of electromagnetic shielding and environmental sealing requirement, can satisfy simultaneously the request for utilization in in-place forming and, the complex structure shield shell small at volume.
Embodiment
Embodiment is described further the present invention below in conjunction with matrix.The embodiment that the present invention gave an example is only as explanation usefulness of the present invention, and protection of the present invention is described with claims and is as the criterion.
Embodiment 1: by following order; (1) the ethenyl blocking YSR 3286 (viscosity is 5000mPas) that earlier under 100 ℃, 575g is contained 40% massfraction WHITE CARBON BLACK mixes continuously stirring 6 hours with 425g LV (2000mPas) ethenyl blocking YSR 3286; (2) add 2050g blended conductive filler material: adding the 290g diameter earlier is 10 μ m; Length is 100 μ m nickel bag thomels; Stir and add 1760g median size 50 μ m-100 μ m nickel coated graphite powders after 20 minutes again for 4 times; The each mixing after 20 minutes adds next batch again, and all conductive filler materials added the last continuously stirring in back 4 hours; (3) treat to add 1.5g suppressor factor (acetylene hexalin) after temperature drops to 40 ℃, divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (4) add 30g linking agent (hydrogen content is 0.8% linear methylhydrogenpolysi,oxane), add at twice, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (5) add 1.5g catalyzer (the Ka Ersite catalyzer of Pt content 4000ppm), divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (6) add 0.5g thixotropic agent (Southern Star company, RHODASURF ROX), disposable adding, stirred 40 ℃ of temperature last intermittence 0.5 hour.Whole process need vacuumizes and guarantees pressure reduction 0.09MPa, and stirring-head 8RPM disperses a 80RPM.Obtain tensile strength greater than 1.8MPa, unit elongation is greater than 95%, and shore a hardness is 72, and resistivity is the single-component Ni-C filled FIP hot sulfurization high-conductivity silicon rubber mixture of 0.07 Ω cm.
Embodiment 2: by following order; (1) the ethenyl blocking YSR 3286 (viscosity is 10000mPas) that earlier under 100 ℃, 525g is contained 40% massfraction WHITE CARBON BLACK mixes continuously stirring 6 hours with 475g LV (viscosity 1000mPas) ethenyl blocking YSR 3286; (2) add 2100g blended conductive filler material; Adding the 300g diameter earlier is 10 μ m; Length is 100 μ m nickel bag thomels; Stir after 20 minutes and to add 1800g median size 50 μ m-100 μ m nickel coated graphite powders again for 4 times, mix after 20 minutes at every turn and add next batch again, all conductive filler materials added afterwards at last continuously stirring 4 hours; (3) treat to add 1g part suppressor factor (acetylene hexalin) after temperature drops to 40 ℃, divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (4) add 28g linking agent (hydrogen content is 0.8% methylhydrogenpolysi,oxane), add at twice, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (5) add 1g catalyzer (the Ka Ersite catalyzer of Pt content 5000ppm), divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (6) add 5g thixotropic agent (Southern Star company, RHODASURF ROX), disposable adding, stirred 40 ℃ of temperature last intermittence 0.5 hour.Whole process need vacuumizes and guarantees pressure reduction 0.09MPa, and stirring-head 4RPM disperses a 57RPM.Obtain tensile strength greater than 2.0MPa, unit elongation is greater than 75%, and shore a hardness is 73, and resistivity is the single-component Ni-C filled FIP hot sulfurization high-conductivity silicon rubber mixture of 0.05 Ω cm.
Embodiment 3: by following order; (1) the ethenyl blocking YSR 3286 (viscosity is 20000mPas) that earlier under 100 ℃, 625g is contained 40% massfraction WHITE CARBON BLACK mixes continuously stirring 6 hours with 375g LV (viscosity 1000mPas) ethenyl blocking YSR 3286; (2) add 1950g blended conductive filler material; Adding the 280g diameter earlier is 7 μ m; Length is 200 μ m nickel bag thomels; Stir after 20 minutes and to add 1670g median size 50 μ m-100 μ m nickel coated graphite powders again for 4 times, mix after 20 minutes at every turn and add next batch again, all conductive filler materials added afterwards at last continuously stirring 4 hours; (3) treat to add 0.5 part of suppressor factor (acetylene hexalin) after temperature drops to 40 ℃, divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (4) add 32 parts of linking agents (hydrogen content is 0.8% methylhydrogenpolysi,oxane), add at twice, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (5) add 2g catalyzer (the Ka Ersite catalyzer of Pt content 3000ppm), divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (6) add 10g thixotropic agent (Southern Star company, RHODASURF ROX), disposable adding, stirred 40 ℃ of temperature last intermittence 0.5 hour.Whole process need vacuumizes and guarantees pressure reduction 0.09MPa, and stirring-head 10RPM disperses a 112RPM.Obtain tensile strength greater than 1.5MPa, unit elongation is greater than 112%, and shore a hardness is 69, and resistivity is the single-component Ni-C filled FIP hot sulfurization high-conductivity silicon rubber mixture of 0.12 Ω cm.Embodiment 4: by following order; (1) the ethenyl blocking YSR 3286 (viscosity is 10000mPas) that earlier under 100 ℃, 625g is contained 26% massfraction WHITE CARBON BLACK mixes continuously stirring 6 hours with 375g LV (viscosity 1000mPas) ethenyl blocking YSR 3286; (2) add 2000g blended conductive filler material; Adding the 285g diameter earlier is 7 μ m; Length is 200 μ m nickel bag thomels; Stir after 20 minutes and to add 1715g median size 50 μ m-100 μ m nickel coated graphite powders again for 4 times, mix after 20 minutes at every turn and add next batch again, all conductive filler materials added afterwards at last continuously stirring 4 hours; (3) treat to add 0.5 part of suppressor factor (acetylene hexalin) after temperature drops to 40 ℃, divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (4) add 64 parts of linking agents (hydrogen content is 0.4% methylhydrogenpolysi,oxane), add at twice, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (5) add 1.5g catalyzer (the Ka Ersite catalyzer of Pt content 3000ppm), divide 2 addings, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour; (6) add 8g thixotropic agent (Southern Star company, RHODASURF ROX), disposable adding, stirred 40 ℃ of temperature last intermittence 0.5 hour.Whole process need vacuumizes and guarantees pressure reduction 0.09MPa, and stirring-head 10RPM disperses a 112RPM.Obtain tensile strength greater than 1.9MPa, unit elongation is greater than 85%, and shore a hardness is 70, and resistivity is the single-component Ni-C filled FIP hot sulfurization high-conductivity silicon rubber mixture of 0.10 Ω cm.

Claims (1)

1. the high conductive silicon compounded rubber of single-component Ni-C filled FIP hot sulfurization is characterized in that, comprise that following material component prepares: (1) 52.5-62.5 weight part contains the ethenyl blocking YSR 3286 of WHITE CARBON BLACK; (2) the LV ethenyl blocking YSR 3286 of 37.5-47.5 weight part; (3) 195-210 weight part Ni-C conductive filler material; (4) 0.1-0.15 weight part alkynol suppressor factor; (5) the linear methylhydrogenpolysi,oxane linking agent of 2.8-3.2 weight part Si-H base, hydrogen matrix amount per-cent 0.4-0.8%; (6) the Ka Ersite platinum catalyst of 0.1-0.2 weight part, Pt content 3000-5000ppm; (7) thixotropic agent of 0.05-1 weight part;
(1) the ethenyl blocking YSR 3286 of WHITE CARBON BLACK in, the content of WHITE CARBON BLACK is 20%-40%, and the viscosity of ethenyl blocking YSR 3286 is 5000-20000mPas, and the vinyl mass percent is 0.26%-0.28%; (2) LV ethenyl blocking YSR 3286 is that viscosity is one or more LV ethenyl blocking YSR 3286s of 1000-2000mPas in, and contents of ethylene is 0.7%-0.8%; (3) the Ni-C conductive filler material described in is meant nickel coated graphite powder and nickel bag thomel; The Ni-C conductive filler material of nickel coated graphite powder and nickel bag thomel is that nickel coated graphite powder and the 28-30 part diameter of 167-180 part median size 50 μ m-100 μ m is that 7-10 μ m, length are the nickel bag thomel of 100-200 μ m;
Its preparation method may further comprise the steps:
1. mix with LV ethenyl blocking YSR 3286 at 100 ℃ of ethenyl blocking YSR 3286s that will contain WHITE CARBON BLACK down, vacuumize assurance pressure reduction >=0.09MPa, continuously stirring 4-6 hour, stirring-head 4-10RPM disperseed a 57-114RPM;
2. the Ni-C conductive filler material that on basis 1., adds nickel coated graphite powder and nickel bag thomel: add nickel bag thomel earlier; Add remaining nickel coated graphite powder more in batches, mix after 20-30 minute at every turn and add next batch again, last continuously stirring 4-6 hour; 100 ℃ of temperature; Vacuumize assurance pressure reduction >=0.09MPa, stirring-head 4-10RPM disperses a 57-114RPM;
3. on basis 2., add suppressor factor, add in batches, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour, 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM;
4. on basis 3., add linking agent, add in batches, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour, 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM;
5. on basis 4., add catalyzer, add in batches, mix after 5 minutes at every turn and add next batch again, last continuously stirring 1 hour, 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM;
6. on basis 5., add thixotropic agent, disposable adding, stirred 0.5 hour last intermittence, and 40 ℃ of temperature vacuumize assurance pressure reduction >=0.09MPa, and stirring-head 4-10RPM disperses a 57-114RPM.
According to the compounded rubber of claim 1, it is characterized in that 2, the alkynol suppressor factor described in (4) is the acetylene hexalin.
CN2011101520743A 2011-06-08 2011-06-08 Mono-component Ni-C filled-type FIP (Form In Place) heat-curing highly-conductive silicone rubber and preparation method thereof Expired - Fee Related CN102276988B (en)

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CN106976188A (en) * 2016-01-18 2017-07-25 深圳市海德讯科技有限公司 Thermal transfer conducting resinl pads forming method in a kind of high-accuracy mould
CN107069046A (en) * 2017-04-27 2017-08-18 中国科学院宁波材料技术与工程研究所 A kind of metal air battery cathodes and preparation method thereof, metal-air battery
CN110003664A (en) * 2019-04-15 2019-07-12 深圳市威富通讯技术有限公司 Liquid conductive silastic and its preparation method and application
CN113604192A (en) * 2021-08-31 2021-11-05 广州市白云化工实业有限公司 High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof
CN114479467A (en) * 2021-12-18 2022-05-13 航天长屏科技有限公司 Ultra-soft high-resilience electromagnetic shielding rubber and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4545914A (en) * 1984-08-31 1985-10-08 Dow Corning Corporation Conductive elastomers from electrically conductive fibers in silicone emulsion
JP2003059341A (en) * 2001-08-10 2003-02-28 Shin Etsu Chem Co Ltd Conductive silicone rubber composition
JP2004155949A (en) * 2002-11-07 2004-06-03 Kitagawa Ind Co Ltd Electroconductive and heat conductive sheet and its preparation method
CN1528000A (en) * 2001-04-06 2004-09-08 ����Ʋ��ɷ����޹�˾ Electrically conductive silicones and method of manufacture thereof
CN1775862A (en) * 2005-09-16 2006-05-24 上海锐朗光电材料有限公司 Single-component room-temperature curable nigh conductive silicon rubber composition
CN101624471A (en) * 2009-03-06 2010-01-13 上海锐朗光电材料有限公司 Heat curing in-situ forming high-conductivity silicon rubber composition and application thereof
CN102010600A (en) * 2010-11-26 2011-04-13 广州天赐有机硅科技有限公司 Conductive liquid silicon rubber-based adhesive and preparation method for composition thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59199756A (en) * 1983-04-27 1984-11-12 Toshiba Silicone Co Ltd Conductive silicone rubber composition
US20020022136A1 (en) * 2000-08-21 2002-02-21 Valade Joseph A. Conductive curable composition

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4545914A (en) * 1984-08-31 1985-10-08 Dow Corning Corporation Conductive elastomers from electrically conductive fibers in silicone emulsion
CN1528000A (en) * 2001-04-06 2004-09-08 ����Ʋ��ɷ����޹�˾ Electrically conductive silicones and method of manufacture thereof
JP2003059341A (en) * 2001-08-10 2003-02-28 Shin Etsu Chem Co Ltd Conductive silicone rubber composition
JP2004155949A (en) * 2002-11-07 2004-06-03 Kitagawa Ind Co Ltd Electroconductive and heat conductive sheet and its preparation method
CN1775862A (en) * 2005-09-16 2006-05-24 上海锐朗光电材料有限公司 Single-component room-temperature curable nigh conductive silicon rubber composition
CN101624471A (en) * 2009-03-06 2010-01-13 上海锐朗光电材料有限公司 Heat curing in-situ forming high-conductivity silicon rubber composition and application thereof
CN102010600A (en) * 2010-11-26 2011-04-13 广州天赐有机硅科技有限公司 Conductive liquid silicon rubber-based adhesive and preparation method for composition thereof

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