CN102276988A - 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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CN102276988A
CN102276988A CN2011101520743A CN201110152074A CN102276988A CN 102276988 A CN102276988 A CN 102276988A CN 2011101520743 A CN2011101520743 A CN 2011101520743A CN 201110152074 A CN201110152074 A CN 201110152074A CN 102276988 A CN102276988 A CN 102276988A
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ethenyl blocking
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CN102276988B (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-type 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-type 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 electromagnetic interference 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 to human and other organism.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 through being processed into design, by 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.
Miniaturization along with electronics, as mobile phone, palm PC (Personal Digital Assistant, PDA), PC (Personal Computer, PC) card etc., conventional conductive rubber is subjected to actual production technique and manufacturing cost restriction, can't satisfy the service requirements 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 by 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.High viscosity 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 save cost.Traditional processing 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 forms liner and substrate forms permanent bonding under heating, and working method is simple.Traditional conductive rubber also needs to assemble groove and the positioning screw hole that matches with washer-shaped, has increased time of setting-up and manufacturing cost.And by regulating Glue dripping head internal diameter size and putting the adhesive tape that glue laminated power 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 automatization 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, can be accurate and exactly the colloid point of shape unanimity is applied to that original position is shaped on the specified small flange surface, satisfied the demand of in enormous quantities and rapid growth 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) announced that a kind of is that the mode of 10-150 μ m conductive particle has prepared the in-place forming conductive silicon rubber by add 100-500 weight part particle size in the ethenyl blocking polydimethylsiloxane; 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 is when too many; not only increased material cost; 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 polydimethylsiloxane of 50000mPa.s viscosity, volume specific resistance just is 0.008 Ω cm when silver-coated copper powder end addition reaches 400 weight parts as patent CN101624471A example 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 by 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 example 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 composition 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 matrix 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 matrix+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: also there are the following problems and difficulty does not overcome for conductive silicon oxyalkyl matrix material 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 use in 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-type 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-type 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 polydimethylsiloxane of white carbon black; (2) the low viscosity ethenyl blocking polydimethylsiloxane 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 inhibitor; (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 carbon fiber.Be applied to require the electromagnetic shielding of in-place forming and the electronics of environmental sealing.
The ethenyl blocking polydimethylsiloxane of white carbon black in (1) wherein, the content of white carbon black is 20%-40%, and the viscosity of ethenyl blocking polydimethylsiloxane is 5000-20000mPas, and the vinyl mass percent is 0.26%-0.28%.
(2) low viscosity ethenyl blocking polydimethylsiloxane in, the low viscosity ethenyl blocking polydimethylsiloxane 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 carbon fiber are 7-10 μ m in, and length is the nickel bag carbon fiber of 100-200 μ m.
(4) the alkynol inhibitor 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-type FIP hot sulfurization may further comprise the steps:
(1) mix with low viscosity ethenyl blocking polydimethylsiloxane at 100 ℃ of ethenyl blocking polydimethylsiloxanes 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 carbon fiber on the basis of (1): add nickel bag carbon fiber earlier, add remaining nickel coated graphite powder more in batches, the each mixing after 20-30 minute adds 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 inhibitor, 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 to coat one deck nickel metal on the carbon material of the relative metal difference of electroconductibility; 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 adjacent electrochondria, produces autoelectronic current.Form conductive network.When forming conductive network by first kind of mechanism, the electroconductibility of conductive rubber just can be fine, and the adding of nickel bag carbon fiber can make the probability that particle is in contact with one another become big under the situation that contains the identical weight umber, thereby easier formation conductive path obtains the material that meets of good conductivity.Can obtain single-component Ni-C filled-type FIP hot sulfurization high-conductivity silicon rubber by 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, silicon rubber is typical non-Newtonian fluid, the temperature low more characteristic of high viscosity is more arranged, therefore 100 ℃ of viscosity that can effectively reduce silicon rubber down, make that the conductive filler material dispersive is more even.Can remove the organic molecule that remains in the silicon rubber under this temperature simultaneously, these small molecules are that organic products produces in preparation process.Residual small molecules can make conductive rubber produce pore when sulfuration.The fusing point of acetylene hexalin is 30-33 ℃, need mix down at 40 ℃ when room temperature is lower, can prevent the crystallization of inhibitor acetylene hexalin, avoids the inhibitor skewness.Vacuum condition helps to be adsorbed on overflowing of gas on the conductive filler material, and these gases can make conductive rubber produce pore when sulfuration.Thixotropic agent can form effective three-dimensional network by 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 fracture of formation 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, inhibitor will add before linking agent and catalyzer, the situation that spot cure only after the inhibitor thorough mixing is even, just can not occur, because when not having inhibitor, 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 inhibitor, the low excessively inhibitor 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 carbon fiber 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) by preparation technology and additive, make glue have good flowability and thixotropic property, can satisfy the service requirements 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 service requirements in in-place forming and, the complex structure shield shell small at volume.
Embodiment
The invention will be further described below in conjunction with matrix embodiment.The embodiment that the present invention exemplified usefulness only of the present invention as an illustration, protection of the present invention are described with claims and are as the criterion.
Embodiment 1: in the following order, (1) the ethenyl blocking polydimethylsiloxane (viscosity is 5000mPas) that 575g is contained earlier 40% massfraction white carbon black under 100 ℃ mixes continuously stirring 6 hours with 425g low viscosity (2000mPas) ethenyl blocking polydimethylsiloxane; (2) add 2050g blended conductive filler material: adding the 290g diameter earlier is 10 μ m, length is 100 μ m nickel bag carbon fibers, 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 inhibitor (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-type FIP hot sulfurization high-conductivity silicon rubber mixture of 0.07 Ω cm.
Embodiment 2: in the following order, (1) the ethenyl blocking polydimethylsiloxane (viscosity is 10000mPas) that 525g is contained earlier 40% massfraction white carbon black under 100 ℃ mixes continuously stirring 6 hours with 475g low viscosity (viscosity 1000mPas) ethenyl blocking polydimethylsiloxane; (2) add 2100g blended conductive filler material, adding the 300g diameter earlier is 10 μ m, length is 100 μ m nickel bag carbon fibers, stir and add 1800g 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 1g part inhibitor (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-type FIP hot sulfurization high-conductivity silicon rubber mixture of 0.05 Ω cm.
Embodiment 3: in the following order, (1) the ethenyl blocking polydimethylsiloxane (viscosity is 20000mPas) that 625g is contained earlier 40% massfraction white carbon black under 100 ℃ mixes continuously stirring 6 hours with 375g low viscosity (viscosity 1000mPas) ethenyl blocking polydimethylsiloxane; (2) add 1950g blended conductive filler material, adding the 280g diameter earlier is 7 μ m, length is 200 μ m nickel bag carbon fibers, stir and add 1670g 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 0.5 part of inhibitor (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-type FIP hot sulfurization high-conductivity silicon rubber mixture of 0.12 Ω cm.Embodiment 4: in the following order, (1) the ethenyl blocking polydimethylsiloxane (viscosity is 10000mPas) that 625g is contained earlier 26% massfraction white carbon black under 100 ℃ mixes continuously stirring 6 hours with 375g low viscosity (viscosity 1000mPas) ethenyl blocking polydimethylsiloxane; (2) add 2000g blended conductive filler material, adding the 285g diameter earlier is 7 μ m, length is 200 μ m nickel bag carbon fibers, stir and add 1715g 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 0.5 part of inhibitor (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-type FIP hot sulfurization high-conductivity silicon rubber mixture of 0.10 Ω cm.

Claims (5)

1. the high conductive silicon compounded rubber of single-component Ni-C filled-type FIP hot sulfurization is characterized in that comprise following material: (1) 52.5-62.5 weight part contains the ethenyl blocking polydimethylsiloxane of white carbon black; (2) the low viscosity ethenyl blocking polydimethylsiloxane 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 inhibitor; (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 carbon fiber.
2. according to the compounded rubber of claim 1, it is characterized in that, (1) the ethenyl blocking polydimethylsiloxane of white carbon black in, the content of white carbon black is 20%-40%, the viscosity of ethenyl blocking polydimethylsiloxane is 5000-20000mPas, and the vinyl mass percent is 0.26%-0.28%; (2) low viscosity ethenyl blocking polydimethylsiloxane in, the low viscosity ethenyl blocking polydimethylsiloxane of one or more different viscosity, viscosity is 1000-2000mPas, contents of ethylene is 0.7%-0.8%.
3. according to the compounded rubber of claim 1, it is characterized in that, (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 carbon fiber are 7-10 μ m in, and length is the nickel bag carbon fiber of 100-200 μ m.
4. according to the compounded rubber of claim 1, it is characterized in that the alkynol inhibitor described in (4) is the acetylene hexalin.
5. according to the preparation method of the high conductive silicon compounded rubber of a kind of single-component Ni-C filled-type FIP hot sulfurization of claim 1, it is characterized in that, may further comprise the steps:
(1) mix with low viscosity ethenyl blocking polydimethylsiloxane at 100 ℃ of ethenyl blocking polydimethylsiloxanes 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 carbon fiber on the basis of (1): add nickel bag carbon fiber earlier, add remaining nickel coated graphite powder more in batches, the each mixing after 20-30 minute adds 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 inhibitor, 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.
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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CN103496228A (en) * 2013-08-29 2014-01-08 北京工业大学 Structural conductive silicone rubber for electromagnetic shielding and preparation
TWI476276B (en) * 2012-12-27 2015-03-11
CN104530718A (en) * 2014-12-27 2015-04-22 北京工业大学 Intelligent conductive composite material and preparation method thereof
WO2017114440A1 (en) * 2015-12-31 2017-07-06 Bluestar Silicones Shanghai Co., Ltd. Electrically-conductive curable organosilicon rubber
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

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TWI476276B (en) * 2012-12-27 2015-03-11
CN103496228A (en) * 2013-08-29 2014-01-08 北京工业大学 Structural conductive silicone rubber for electromagnetic shielding and preparation
CN103496228B (en) * 2013-08-29 2016-07-13 北京工业大学 A kind of electromagnetic shielding structural conductive silicone rubber and preparation
CN104530718A (en) * 2014-12-27 2015-04-22 北京工业大学 Intelligent conductive composite material and preparation method thereof
CN104530718B (en) * 2014-12-27 2017-02-22 北京工业大学 Intelligent conductive composite material and preparation method thereof
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US10822473B2 (en) 2015-12-31 2020-11-03 Elkem Silicones Shanghai Co., Ltd. Electrically-conductive curable organosilicon rubber
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

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