CN102382616B - Dual components condensed type room temperature cured high conductive silicone rubber adhesive and application method thereof - Google Patents
Dual components condensed type room temperature cured high conductive silicone rubber adhesive and application method thereof Download PDFInfo
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Abstract
The invention provides a dual components condensed type room temperature cured high conductive silicone rubber adhesive. The adhesive is divided into a component A and a component B. The component A is composed of a metal-based conductive filling material, a hydroxy terminiated polysiloxanes mixture and a catalyst; the components B is composed of the metal-based conductive filling material, the hydroxy terminiated polysiloxanes mixture and a curing agent. The invention has the advantages that the conductive performance is excellent, the solidification process is not influenced by the glue layer thickness, the phenomenon of catalyst poisoning is not generated, the conductivity is high, the cohesiveness and the sealing are strong, the elasticity is good and the application scope is wide. The adhesive is used for bonding metal, semiconductor, ITO electro-conductive glass and the like to form a conductive-sealant integral body, especially used for package application of a AB rubber pipe. The invention also provides an application method of the silicone rubber adhesive. The method comprises the following steps: fully mixing the component A and the component B according to ratio of 1:1, curing and molding under the room temperature condition. The method has the advantages of room temperature solidification, no requirement of water and gas absorption, deep solidification realization and dual components ratio with 1:1, and is convenient for package application of the AB rubber pipe.
Description
Technical field
The invention belongs to chemical material technical field, specifically a kind of Dual components condensed type room temperature cured high conductive silicone rubber adhesive and preparation method thereof.
Background technology
Along with the development of electronic industry, the electromagnetic shielding of electronic circuit is more and more come into one's own.A large amount of radio products, such as mobile phone, GPS navigation instrument, wireless network card etc. all can produce electromagnetic radiation, causes interference to the inner normal signal of other electronic systems, and also ecotope threatens to external world.Generally adopt and electronic circuit package is formed in external conductive casing to the integral body of electromagnetic shielding for this reason.But in slab joint place of shell, usually because causing shielding, poorly conductive declines.Need, by certain method, these seams are coupled together to improve shielding properties with the material seal of high conduction for this reason.
Conductive silicon rubber is as a kind of novel matrix material, has advantages of that electroconductibility is high, good springiness, long service life, is widely used in the connection of electromagnetic shielding box, shielding case seam crossing.Traditional application mode is generally first to make conductive silicon rubber bar, then is pressed on seam crossing.Such as Chinese patent: CN1605604 discloses a kind of conductive silicon rubber composition, adopt the mode of mixing two-component silicone rubber and silver-plated conductive particle filler, technique (100 ~ 250 degrees Celsius of thermal treatment temps) by hot briquetting, obtains high-conductivity silicon rubber bar.Chinese patent: CN1649963 adopts metal matrix conductive filler material and spherical silicone rubber particles as the weighting material of addition-type silicon rubber, vulcanizes high-conductivity silicon rubber sheet or the India-rubber strip that has obtained soft and low permanent compression set under 150 degrees Celsius of conditions of two hours.But such method application is very dumb, need in many instances the conductive silicon rubber bar of specified shape customized could meet the requirement of electromagnetic shielding.For this reason, people wish to develop and a kind ofly can first inject seam crossing, more curing conductive silicon rubber tackiness agent, meet the electromagnetic shielding demand of different occasions.
The conductive silicon rubber tackiness agent of self-vulcanizing can meet above demand.This is a kind ofly before use for high viscosity liquid, to be injected into after seam, at room temperature places for some time, just can be cured as highly conduct electricity, flexible, long-life conductive silicon rubber, and can be connected with the material on seam both sides closely.
Our company's disclosed patent application recently, having developed a kind of room temperature can deep layer solidify in-situ forming high-conductivity silicon rubber tackiness agent.This is the curing conductive silicon rubber of a kind of room temperature add-on type, has solved smoothly the curing difficult problem of conductive silicon rubber room temperature deep layer, has obtained good effect in practical application.But due to the catalyzer of addition-type silicon rubber employing platiniferous, the material that is easily contained the elements such as nitrogen phosphate and sulfur, tin by some is poisoning.Catalyzer after poisoning has just lost activity, causes solidifying difficulty.Therefore in some occasion (such as directly contacting bump), cannot apply.
Chinese patent CN1775862 discloses a kind of single-component room-temperature curable nigh conductive silicon rubber composition.Said composition is mixed and is formed by absorbing the curing condensed type room curing silicon rubber (RTV-1) of water in air steam and metal matrix conductive filler material and functional stuffing.During use, from the sealed vessel of isolated moisture, take out, be coated in the joint face place that needs connection, by being exposed to from airborne aqueous vapor, be solidified into target conductive silicon rubber composition.But this conductive silicon rubber is curing by absorbing airborne aqueous vapor, therefore there is the common shortcoming of all RTV-1 silicon rubber, be exactly deep layer to solidify.When bondline thickness surpasses 3mm, inside will be solidified slowly and even can not be solidified.
Therefore, developing a room temperature of not being afraid of poisoning of catalyst can deep layer solidify the condensed type high-conductivity silicon rubber tackiness agent of in-place forming and becomes a new requirement, and at room temperature can there is longer working life for this condensed type high-conductivity silicon rubber tackiness agent, generally need to be designed to two components, high-conductivity silicon rubber for two components, be preferably made the ratio of 1:1, and two component viscosity, density are close.So just can make with the two sebific ducts of AB and pack and use AB glue rifle and mixing tube to extrude the product of use, be convenient to flexible Application.
Reference:
CN 1605604 high electroconductive rubbers and manufacture method thereof
CN 1649963 conductive silicon rubber compositions
CN 1775862 single-component room-temperature curable nigh conductive silicon rubber compositions.
Summary of the invention
The object of the invention is in order to overcome the deficiencies in the prior art a kind of Dual components condensed type room temperature cured high conductive silicone rubber adhesive of design.
For this reason, the present invention adopts following technical scheme: this tackiness agent is divided into A, two components of B.A component is: metal matrix conductive filler material, the mixture of hydroxy-end capped polysiloxane, catalyzer; B component is: metal matrix conductive filler material, the mixture of hydroxy-end capped polysiloxane, solidifying agent.
By above technical scheme, conductivity of the present invention is good, and solidification process do not affect by bondline thickness, there is no poisoning of catalyst phenomenon, and electroconductibility is high, and cohesiveness and stopping property are strong, good springiness, applied range.For matrix metal, semi-conductor, ITO conductive glass etc., form the integral body of conductive seal.Be specially adapted to the packaging application of the two sebific ducts of AB.
The present invention also comprises the using method of above-mentioned silicone rubber adhesive, and described method is for fully to mix A, B component according to the ratio of 1:1, at ambient temperature curing molding.
Present method has the following advantages: self-vulcanizing, do not need to absorb aqueous vapor, and can realize deep layer and solidify; Two-pack 1:1 proportioning, is convenient to AB sebific duct packing and uses.
Accompanying drawing explanation
Curing speed and the room temperature storage phase comparison sheet of the different solidifying agent of Fig. 1.
Embodiment
The invention belongs to chemical material technical field, specifically a kind of Dual components condensed type room temperature cured high conductive silicone rubber adhesive and preparation method thereof.
In the making of electromagnetic shielding equipment, need high-conductivity silicon rubber.Traditional conductive silicon rubber bar is used underaction.And existing conductive silicon rubber that can be at room temperature curing exists and is difficult to realize that deep layer is solidified or the problem of poisoning of catalyst.Therefore developing a room temperature of not being afraid of poisoning of catalyst can deep layer solidify the high-conductivity silicon rubber tackiness agent of in-place forming and becomes a new requirement.
The present invention has prepared the conductive silicon rubber of a kind of pair of component, and it is mainly by metal matrix conductive filler material, the mixture of the hydroxy-end capped polysiloxane of certain viscosity, and catalyzer, functional stuffing, solidifying agent forms.During use, A, B component are evenly mixed according to the ratio of 1:1, be coated on the joint face that needs conduction bonding, after self-vulcanizing, form high-conductivity silicon rubber elastomerics.Be specially adapted to the packaging application of the two sebific ducts of AB.
This tackiness agent is divided into A, two components of B.A component is: metal matrix conductive filler material, the mixture of hydroxy-end capped polysiloxane, catalyzer; B component is: metal matrix conductive filler material, the mixture of hydroxy-end capped polysiloxane, solidifying agent.
In described A component, the weight ratio of metal matrix conductive filler material, hydroxy-end capped polysiloxane, catalyzer is: 700 ~ 1000:100:1 ~ 10.
In described B component, the weight ratio of metal matrix conductive filler material, hydroxy-end capped polysiloxane, solidifying agent is: 700 ~ 1000:100:5 ~ 20.
Described B component also comprises functional stuffing, and the weight ratio of described functional stuffing and metal matrix conductive filler material, hydroxy-end capped polysiloxane, solidifying agent is: 0 ~ 10:700 ~ 1000:100:5 ~ 20.
The mixture of described hydroxy-end capped polysiloxane, its hydroxy radical content is 0.04% ~ 0.10%, viscosity is 1000 ~ 10000cp.
Described functional stuffing is thermal silica or tackifier or water-resisting agent or their mixture.
Described catalyzer is organo-tin compound or organic titanic compound.
Described solidifying agent is that structural formula is R-Si (OC
2h
5)
3compound, wherein R is methyl, phenyl, oxyethyl group or vinyl.
The particle diameter of above-described metal matrix conductive filler material, at 200nm ~ 5000nm, is shaped as sheet or spherical or dendroid, and material is silver powder, nickel powder, copper powder or silver-plated glass powder or silver-plated copper powder, nickel powder.
The detailed description of each compositional selecting:
Metal matrix conductive filler material: major function is to be filled in silicon rubber base material is realized electroconductibility after solidifying.According to the theory of conductive resin, it is because some mutual close contact has formed conductive path between inner metal matrix conductive filler particles of filling that conductive silicon rubber can conduct electricity.This just needs two conditions: the firstth, and it is enough many that metal matrix conductive filler particles quantity is wanted, and making between them can close contact; Another is that the contact between metal matrix conductive filler particles is conductive contact, and should there be insulation layer on their surface.In general, more or less all can there be certain surface group on metal matrix conductive filler particles surface, such as zone of oxidation, and tensio-active agent etc.Therefore to select the metal matrix conductive filler particles of surface conduction.Such as the powder of silver, nickel, copper, or at the conductive powder of glass micro mist, copper powder, nickel powder electroplate gained.Their shape also has a certain impact for electroconductibility.In general, spherical micro mist comparison can be piled up closely, but the area of contact few mutually.Sheet or dendritic micro mist, the density of accumulation is not as spherical, but mutually, the area of contact is not little.Sheet and dendritic micro mist in addition, the conductive resin viscosity of filling can be larger, and this easily causes not as ball-shaped micro powder owing to being subjected to displacement between filler.
The mixture of the hydroxy-end capped polysiloxane of certain viscosity: its function is the base polymer of silicon rubber, after it and solidifying agent, catalyst mix, can solidify to form silicon rubber base material.Simultaneously also as the dispersion agent of uncured glue, provide can be mobile performance.Its chemical constitution can be used general formula: HO-[Si (CH
3)
2o]
n-H expresses.N=450 ~ 1000 wherein, corresponding hydroxy radical content is 0.10% ~ 0.04%, viscosity is 1000 ~ 10000cp.Hardness and the tensile strength of the silicon rubber of the mixture gained of the hydroxy-end capped polysiloxane of different viscosity are different.When the viscosity of the mixture of hydroxy-end capped polysiloxane is 1000cp, the hardness that obtains conductive silicon rubber is Shao Shi A70, the about 3.2MPa of intensity; When the viscosity of the mixture of hydroxy-end capped polysiloxane is 10000cp, the hardness that obtains conductive silicon rubber is Shao Shi A55, the about 3.9MPa of intensity.By regulating the viscosity of the mixture of hydroxy-end capped polysiloxane, can be so that this product be used the physicals of front and back to reach optimum.
Functional stuffing: its function is to give conductive silicon rubber cohesiveness, higher intensity, water-repellancy etc.Mainly contain thermal silica, can improve intensity; Silane coupling agent KH-560(3-(2,3 epoxy the third oxygen) propyl trimethoxy silicane), can improve cohesiveness; Calcium carbonate fine powder, can improve water-repellancy.The amount of functional stuffing is too much unsuitable, otherwise can affect electroconductibility and other mechanical propertys of conductive silicon rubber.
Catalyzer: its function is to accelerate the speed of response of hydroxy-end capped polysiloxane and solidifying agent, and the time of self-vulcanizing is shortened.Be mainly organo-tin compound or organic titanic compound.As: dibutyltin diacetate, dibutyl tin laurate, two dioctyltin laurate, two (second-thylhexoic acid) dibutyl tin, diisooctyl toxilic acid dibutyl tin, stannous octoate, the sub-tin of neodecanoic acid, dibutyl tin (beta-diketo-ester); Tetrabutyl titanate, isopropyl titanate, two (methyl aceto acetate) title complexs of 1,3-the third dioxy base titanium.This type of catalyzer can be not poisoning, therefore can be widely used in the various occasions that need conductive shield sealing.
Solidifying agent: its function is to form network-like macromolecular elastomer with hydroxy-end capped polysiloxane reaction.Being mainly structural formula is R-Si (OC
2h
5)
3.Wherein R is methyl, phenyl, oxyethyl group or vinyl.The selection of solidifying agent is very large for the performance impact of conductive silicon rubber.Be mainly manifested on the room temperature storage phase and self-vulcanizing speed of conductive silicon rubber.When R is oxyethyl group, curing speed is the fastest, but the room temperature storage phase is also shorter.When R is followed successively by methyl, vinyl, phenyl, set time and room temperature storage phase all can extend accordingly, reference table 1.The another one way that improves the shelf lives is to adopt cryopreservation.When uncured conductive resin stores under 0 degree Celsius, the shelf lives is than 2 ~ 3 times of length under room temperature.
The present invention also provides the using method of above tackiness agent, and described method is for fully to mix A, B component according to the ratio of 1:1, at ambient temperature curing molding.
Specifically, the A mixing, B component are existed respectively in the container of sealing, during use, A, B component are fully mixed according to the ratio of weight or volume ratio 1:1, be coated on the joint face that needs conduction bonding, self-vulcanizing forms high-conductivity silicon rubber elastomerics for 18 ~ 72 hours.The A preparing according to the present invention, B component high-conductivity silicon rubber, is particularly suitable for adopting the two sebific duct packings of AB, and adopts AB glue rifle and mixing tube to extrude use, flexible and convenient to use.The integral body that forms conductive seal for matrix metal, semi-conductor, ITO conductive glass etc., is widely used in electromagnetic shielding and the sealing of various electronic apparatus shell seam crossings.
Example 1:
The making of A component: in dry, clean container, evenly mix following component: the spherical copper powder that 1000 weight part diameters are 1000nm, the viscosity of 100 weight parts is the mixture of 1000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.10%, the dibutyltin diacetate catalyzer of 10 weight parts.After having mixed, obtain the thick liquid that viscosity is 100000cp ~ 150000cp, be kept in the container of sealing.
The making of B component: in dry, clean container, evenly mix following component: the spherical copper powder that 1000 weight part diameters are 1000nm, the viscosity of 100 weight parts is the mixture of 1000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.10%, the gas-phase silica of 10 weight parts, the Union carbide A-162 solidifying agent of 10 weight parts.After having mixed, obtain the thick liquid that viscosity is 100000cp ~ 150000cp, be kept in the container of sealing.
During use, A, B component are fully mixed to rear use according to the ratio of weight or volume ratio 1:1.1 hour operating time, it is Shao Shi A70 that self-vulcanizing obtains hardness for 26 hours, extensibility 20%, and electric conductivity is less than the high-conductivity silicon rubber of 0.01 ohmcm, at-20 degrees Celsius, to 100 degree celsius temperature, change and do not ftracture, remain good electroconductibility and stopping property.
Example 2:
The making of A component: in dry, clean container, evenly mix following component: the flake silver powder that 700 weight part diameters are 5000nm, the viscosity of 100 weight parts is the mixture of 10000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.04%, the dibutyltin dilaurate catalyst of 1 weight part.After having mixed, obtain the thick liquid that viscosity is 80000cp ~ 120000cp, be kept in the container of sealing.
The making of B component: in dry, clean container, evenly mix following component: the flake silver powder that 700 weight part diameters are 5000nm, the viscosity of 100 weight parts is the mixture of 10000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.04%, do not add functional stuffing, the tetraethoxy solidifying agent of 20 weight parts.After having mixed, obtain the thick liquid that viscosity is 80000cp ~ 120000cp, be kept in the container of sealing.
During use, A, B component are fully mixed to rear use according to the ratio of weight or volume ratio 1:1.40 minutes operating times, it is Shao Shi A55 that self-vulcanizing obtains hardness for 18 hours, extensibility 50%, and electric conductivity is less than the high-conductivity silicon rubber of 0.05 ohmcm, at-20 degrees Celsius, to 100 degree celsius temperature, change and do not ftracture, remain good electroconductibility and stopping property.
Example 3:
The making of A component: in dry, clean container, evenly mix following component: the spherical silvered glass powder that 800 weight part diameters are 200nm, the viscosity of 100 weight parts is the mixture of 3000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.08%, the dibutyl tin of 5 weight parts (beta-diketo-ester) catalyzer.After having mixed, obtain the thick liquid that viscosity is 150000cp ~ 190000cp, be kept in the container of sealing.
The making of B component: in dry, clean container, evenly mix following component: the spherical silvered glass powder that 800 weight part diameters are 200nm, the viscosity of 100 weight parts is the mixture of 3000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.08%, the KH-560 of 5 weight parts, the thermal silica of 5 weight parts, the vinyltriethoxysilane solidifying agent of 5 weight parts.After having mixed, obtain the thick liquid that viscosity is 150000cp ~ 190000cp, be kept in the container of sealing.
During use, A, B component are fully mixed to rear use according to the ratio of weight or volume ratio 1:1.3 hours operating times, it is Shao Shi A63 that self-vulcanizing obtains hardness for 48 hours, extensibility 40%, and electric conductivity is less than the high-conductivity silicon rubber of 0.02 ohmcm, at-20 degrees Celsius, to 100 degree celsius temperature, change and do not ftracture, remain good electroconductibility and stopping property.
Example 4:
The making of A component: in dry, clean container, evenly mix following component: the dendroid nickel powder that 900 weight part diameters are 2000nm, the viscosity of 100 weight parts is the mixture of 5000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.05%, the tetrabutyl titanate catalyzer of 6 weight parts.After having mixed, obtain the thick liquid that viscosity is 120000cp ~ 160000cp, be kept in the container of sealing.
The making of B component: in dry, clean container, evenly mix following component: the dendroid nickel powder that 900 weight part diameters are 2000nm, the viscosity of 100 weight parts is the mixture of 5000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.05%, the calcium carbonate fine powder of 8 weight parts, the KH-560 of 2 weight parts, the phenyl triethoxysilane solidifying agent of 10 weight parts.After having mixed, obtain the thick liquid that viscosity is 120000cp ~ 160000cp, be kept in the container of sealing.
During use, A, B component are fully mixed to rear use according to the ratio of weight or volume ratio 1:1.5 hours operating times, it is Shao Shi A65 that self-vulcanizing obtains hardness for 72 hours, extensibility 40%, and electric conductivity is less than the high-conductivity silicon rubber of 0.01 ohmcm, at-20 degrees Celsius, to 100 degree celsius temperature, change and do not ftracture, remain good electroconductibility and stopping property.
Example 5:
The making of A component: in dry, clean container, evenly mix following component: the spherical silver-plated copper powder that 800 weight part diameters are 3000nm, the viscosity of 100 weight parts is the mixture of 2000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.08%, the isopropyl titanate catalyzer of 10 weight parts.After having mixed, obtain the thick liquid that viscosity is 80000cp ~ 110000cp, be kept in the container of sealing.
The making of B component: in dry, clean container, evenly mix following component: the spherical silver-plated copper powder that 800 weight part diameters are 3000nm, the viscosity of 100 weight parts is the mixture of 2000cp, the hydroxy radical content hydroxy-end capped polysiloxane that is 0.08%, the gas-phase silica of 1 weight part, the tetraethoxy solidifying agent of 10 weight parts.After having mixed, obtain the thick liquid that viscosity is 80000cp ~ 110000cp, be kept in the container of sealing.
During use, A, B component are fully mixed to rear use according to the ratio of weight or volume ratio 1:1.40 minutes operating times, it is Shao Shi A68 that self-vulcanizing obtains hardness for 18 hours, extensibility 20%, and electric conductivity is less than the high-conductivity silicon rubber of 0.06 ohmcm, at-20 degrees Celsius, to 100 degree celsius temperature, change and do not ftracture, remain good electroconductibility and stopping property.
Sum up:
Dual components condensed type room temperature cured high conductive silicone rubber adhesive prepared by the present invention, can at room temperature solidify to form conductivity good, has certain elastic silastic material.Be not subject to the impact of thickness, do not have poisoning of catalyst phenomenon, can connect for the conduction at various interfaces simultaneously.This product electroconductibility is high, and cohesive force is strong, long service life, applied range.Can be made as easily the two sebific duct packings of AB, convenient, flexible needs electromagnetic shielding and conducts electricity the occasions that are connected for various.
For reaching illustration purpose; with preferred embodiments narration as above, so it is not in order to limit the present invention for this patent, and any affiliated technical field without departing from the spirit and scope of the present invention; when doing a little change and polishing, so protection scope of the present invention is when being limited with claims.
Claims (4)
1. Dual components condensed type room temperature cured high conductive silicone rubber adhesive, is characterized in that: this tackiness agent is divided into A, two components of B, and A component is: metal matrix conductive filler material, the mixture of hydroxy-end capped polysiloxane, catalyzer; B component is: metal matrix conductive filler material, and the mixture of hydroxy-end capped polysiloxane, solidifying agent, described solidifying agent is that structural formula is R-Si (OC
2h
5)
3compound, wherein R is methyl, phenyl, oxyethyl group or vinyl, the particle diameter of metal matrix conductive filler material is at 200nm ~ 5000nm, be shaped as sheet or spherical or dendroid, material is silver powder, nickel powder, copper powder or silver-plated glass powder or silver-plated copper powder, nickel powder, and the chemical constitution general formula of described hydroxy-end capped polysiloxane is: HO-[Si (CH
3)
2o]
n-H, n=450 ~ 1000 wherein, corresponding hydroxy radical content is 0.10% ~ 0.04%, viscosity is 1000 ~ 10000cP, in described A component, the weight ratio of metal matrix conductive filler material, hydroxy-end capped polysiloxane, catalyzer is: 700 ~ 1000: 100: 1 ~ 10, and in described B component, the weight ratio of metal matrix conductive filler material, hydroxy-end capped polysiloxane, solidifying agent is: 700 ~ 1000: 100: 5 ~ 20.
2. the Dual components condensed type room temperature cured high conductive silicone rubber adhesive as described in claim 1, it is characterized in that described B component also comprises functional stuffing, the weight ratio of described functional stuffing and metal matrix conductive filler material, hydroxy-end capped polysiloxane, solidifying agent is: 0 ~ 10: 700 ~ 1000: 100: 5 ~ 20.
3. according to the Dual components condensed type room temperature cured high conductive silicone rubber adhesive described in claim 2, it is characterized in that described functional stuffing is thermal silica or tackifier or water-resisting agent or their mixture.
4. according to the Dual components condensed type room temperature cured high conductive silicone rubber adhesive described in claim 1, it is characterized in that described catalyzer is organo-tin compound or organic titanic compound.
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