CN105907361B - Single-component room temperature vulcanized conductive silica gel and preparation method thereof - Google Patents
Single-component room temperature vulcanized conductive silica gel and preparation method thereof Download PDFInfo
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- CN105907361B CN105907361B CN201610544122.6A CN201610544122A CN105907361B CN 105907361 B CN105907361 B CN 105907361B CN 201610544122 A CN201610544122 A CN 201610544122A CN 105907361 B CN105907361 B CN 105907361B
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- conductive filler
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 36
- 239000000741 silica gel Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000011231 conductive filler Substances 0.000 claims abstract description 52
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 20
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 8
- 229920002545 silicone oil Polymers 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920001971 elastomer Polymers 0.000 claims abstract description 7
- 239000004945 silicone rubber Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- -1 ethylamine methyl ethoxy silane Chemical compound 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 19
- 239000006185 dispersion Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 229910021485 fumed silica Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000499 gel Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- BTXFTCVNWMNXKH-UHFFFAOYSA-N NC1=CC=CC=C1.CCO[Si](C)(OCC)OCC Chemical compound NC1=CC=CC=C1.CCO[Si](C)(OCC)OCC BTXFTCVNWMNXKH-UHFFFAOYSA-N 0.000 claims description 2
- 229910020388 SiO1/2 Inorganic materials 0.000 claims description 2
- 229910020485 SiO4/2 Inorganic materials 0.000 claims description 2
- KRJRKEPWQOASJN-UHFFFAOYSA-N aniline;trimethoxy(methyl)silane Chemical compound NC1=CC=CC=C1.CO[Si](C)(OC)OC KRJRKEPWQOASJN-UHFFFAOYSA-N 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- IXQMGECVDWVOFK-UHFFFAOYSA-N dichloromethyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C(Cl)Cl IXQMGECVDWVOFK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- UMXXGDJOCQSQBV-UHFFFAOYSA-N n-ethyl-n-(triethoxysilylmethyl)ethanamine Chemical compound CCO[Si](OCC)(OCC)CN(CC)CC UMXXGDJOCQSQBV-UHFFFAOYSA-N 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 abstract description 6
- 230000032683 aging Effects 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 abstract description 3
- 239000010439 graphite Substances 0.000 abstract description 3
- 238000004891 communication Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- SDSJXKVMZWTZMK-UHFFFAOYSA-N chloromethyl(ethoxy)silane Chemical compound ClC[SiH2]OCC SDSJXKVMZWTZMK-UHFFFAOYSA-N 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 230000035939 shock Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 11
- 238000003860 storage Methods 0.000 description 10
- 239000002390 adhesive tape Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- MXLBKVCGLRNKBW-UHFFFAOYSA-N C(=C)OO[Si](C(C)(C)C)(C(C)(C)C)C(C)(C)C Chemical compound C(=C)OO[Si](C(C)(C)C)(C(C)(C)C)C(C)(C)C MXLBKVCGLRNKBW-UHFFFAOYSA-N 0.000 description 1
- BPMGYFSWCJZSBA-UHFFFAOYSA-N C[SiH](C)O[SiH3] Chemical compound C[SiH](C)O[SiH3] BPMGYFSWCJZSBA-UHFFFAOYSA-N 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Conductive Materials (AREA)
Abstract
The single-component room temperature vulcanized conductive silica gel is characterized in that the conductive silica gel is prepared from the following raw materials in parts by weight: silicon rubber-based rubber: a crosslinking agent: conductive filler and treating agent: filler = 100: 10-20: 300-450: 2-3; wherein the weight ratio of the conductive filler to the treating agent is 100: 1 to 2. The silicone rubber base adhesive is the combination of hydroxyl silicone oil and MQ resin, the conductive filler is the combination of silver-plated copper powder, silver powder, nickel-plated graphite and the like, and the cross-linking agent is the combination containing ethylamine methyl ethoxy silane or chloromethyl ethoxy silane. The invention also discloses a preparation method of the single-component room temperature vulcanized conductive silica gel. The conductive silica gel has good conductive and shielding performance, moderate hardness of 40-50 ℃, good aging resistance (-70-200 ℃), good mechanical strength, convenient use, high bonding strength and elasticity, is tightly attached to a contact surface when used for an electronic connecting device, and plays a role in sealing and shock absorption while conducting and shielding. The method is suitable for conductive shielding bonding in the fields of mobile phone communication and the like.
Description
Technical Field
The invention belongs to a conductive shielding material, and particularly relates to high-strength single-component room-temperature vulcanized conductive silica gel and a preparation method thereof.
Background
With the development of science and technology, electromagnetic wave interference increasingly affects the usability and safety of communication equipment such as mobile phones and the like, in order to solve the problem, a conductive material is usually adopted to shield electromagnetic waves, for example, a metal or conductive plastic shell is adopted, but the shielding effect of parts such as joints, bonding points or small holes of the shell and the like is reduced, so that the parts need to use a conductive rubber material with certain elasticity, and conductive silicone rubber with good mechanical property and weather resistance is an ideal choice.
After the silicon rubber material is cured, the shrinkage rate is small, the stress of a glue layer cannot be generated, but the silicon rubber material has insulation property, and the conductivity can be obtained only by adding a certain proportion of conductive fillers, such as carbon black, silver powder, silver-plated copper powder, nickel-plated graphite powder or metal fiber powder. The pure silver powder has good conductivity but higher price, and the silver-plated copper powder and the nickel-plated graphite have relatively low cost, are corrosion-resistant and oxidation-resistant, and have the characteristics of high magnetic conductivity of nickel and high conductivity of silver powder.
The existing conductive silica gel on the market has the following defects:
most of the components are two components, and the components need to be mixed and vulcanized at high temperature before use, so that the efficiency is low. It is difficult to operate with a dispenser.
The colloid has low tensile strength and bonding strength with the substrate.
Many products contain solvents, which cause volatilization and viscosity change to affect the use process, and the adhesiveness with the metal substrate is reduced, and the conductivity and storage stability of the product are reduced during the use process.
The high-strength single-component room temperature vulcanization conductive silica gel provided by the invention is convenient to use and simple to operate, and can be carried out on a dispensing machine. MQ resin and reinforcing filler are added to improve the strength, and a product adopting the curing crosslinking system is well bonded with a metal substrate. The adoption of different conductive fillers has a complementary effect, and higher addition rate and conductivity are provided. The product is simple to prepare, has no three wastes, has good storage property, does not change in conductivity after being stored for 6 months at the temperature of 2-8 ℃, has no solvent volatilization in the curing process, does not generate air holes in an adhesive layer, and does not influence viscosity change.
Disclosure of Invention
The invention provides a high-strength single-component room temperature vulcanized conductive silica gel and a preparation method thereof, aiming at solving the technical problems of the existing conductive silica gel.
The invention provides single-component room temperature vulcanized conductive silica gel which is prepared from the following raw materials in parts by weight:
silicon rubber-based rubber: a crosslinking agent: conductive filler and treating agent: filler 100: 10-20: 300-450: 2-3;
wherein the weight ratio of the conductive filler to the treating agent is 100: 1 to 2.
The invention also provides a preparation method of the single-component room temperature vulcanized conductive silica gel, which comprises the following steps:
step 1: preparation of conductive filler and treating agent
Placing the conductive filler in a metal or ceramic disc, and baking for 1-3 h in an oven at 50 ℃ to remove the water adsorbed in the conductive filler; and putting the conductive filler and the treating agent into a planetary stirrer according to the proportion of the conductive silica gel, and carrying out dispersion stirring for 10-30 min at a stirring speed of 40-100 rpm to obtain the conductive filler and the treating agent.
Step 2: preparation of conductive silicon rubber material
Weighing various raw materials according to the proportion of the conductive silica gel, firstly putting the silicone rubber base gel, the conductive filler, the treating agent and the filler into a planetary stirrer, stirring for 1-3 h at a dispersion rotation speed of 500-2000 rpm under a vacuum degree of-0.1 MPa and a material temperature of 10-30 ℃, adding the cross-linking agent after uniformly stirring, then stirring for 10-20 min under a vacuum degree of-0.1 MPa, subpackaging and discharging after the cross-linking agent is uniformly dispersed, and storing in a refrigerator.
The product is stored by low-temperature refrigeration, the storage temperature is generally controlled to be 2-8 ℃, and the storage period can be as long as 6 months. The prepared finished single-component silica gel is vulcanized at room temperature, the surface drying time is 6-7min, the complete curing time is 12-24h, the operation is simple, the weather resistance is good, the electrical property is good, the volume resistivity is 0.01 omega cm, and the phenomenon of conductivity reduction is avoided after the use. The adhesive property is good, the shearing strength with the aluminum sheet is more than 2.5MPa, the viscosity change is slow, and the stability of the process is ensured.
Detailed Description
The invention provides single-component room temperature vulcanized conductive silica gel which is prepared from the following raw materials in parts by weight:
silicon rubber-based rubber: a crosslinking agent: conductive filler and treating agent: filler 100: 10-20: 300-450: 2-3;
wherein the weight ratio of the conductive filler to the treating agent is 100: 1 to 2.
Wherein the silicone rubber base rubber is the combination of hydroxyl silicone oil and MQ resin, the hydroxyl silicone oil is α, omega-dihydroxy polydimethylsiloxane, the viscosity is preferably 1000-10000cp at 25 ℃, the MQ resin is methyl MQ resin, and M is a single functionality siloxane closed chain link (CH)3)3SiO1/2Q is tetrafunctional siloxane condensation mer SiO4/2And M/Q is 0.8-1.0. The MQ resin has obvious effect of improving the mechanical strength of the product.
The cross-linking agent is prepared by mixing two raw materials of dichloromethyl triethoxysilane, diethylamino methyl triethoxysilane, aniline methyl triethoxysilane and aniline methyl trimethoxysilane. The cross-linking agent has high bonding strength with a base material after being cured and good weather resistance.
The conductive filler is at least one of silver-plated copper powder, flake silver powder, nickel-plated graphite powder and conductive glass beads with the particle size of less than 50 micrometers. The conductive filler is preferably silver-plated copper powder, flake silver powder and nickel-plated graphite. The flake silver powder D90 is less than 5 microns, the particle size of the silver-plated copper powder is less than 50 microns, and the particle size of the nickel-plated graphite powder is less than 50 microns. The matching of the particle size of the conductive filler powder is beneficial to improving the filling amount and the conductivity. The treating agent is at least one of vinyl tri-tert-butyl peroxy silane, aminopropyl triethoxysilane and vinyl triethoxysilane. The addition of the treating agent can improve the compatibility and stability of the conductive filler and the base rubber.
The filler is at least one of fumed silica, precipitated silica and nano-scale titanium dioxide. The preferable fillers are fumed silica and precipitated silica which are used for adjusting the viscosity of the system and improving the mechanical strength.
The filler is preferably hydrophobic fumed silica subjected to surface treatment by dimethyldichlorosiloxane and dimethyldisiloxane, and the specific surface area of the filler is 100-250 m2/g。
In order to make the objects, technical solutions and effects of the present invention more clear, the present invention is further described in detail by the following examples. The specific embodiments described herein are merely illustrative of the invention and are not intended to be limiting.
Example 1
The preparation method of the single-component room temperature vulcanized conductive silica gel comprises the following steps:
step 1: preparation of conductive filler and treating agent
Placing the conductive filler in a metal or ceramic disc, and baking for 1h in an oven at 50 ℃ to remove the moisture adsorbed in the conductive filler; and putting the conductive filler and the treating agent into a planetary stirrer according to the proportion of the conductive silica gel, dispersing and stirring for 30min at the stirring speed of 100rpm to prepare the conductive filler and the treating agent.
Step 2: preparation of conductive silicon rubber material
Weighing various raw materials according to the proportion of the conductive silica gel, putting the hydroxyl silicone oil, the MQ resin, the conductive filler, the treating agent and the filler into a planetary stirrer, stirring for 1h at a dispersion rotation speed of 500rpm at a vacuum degree of-0.1 MPa and at a material temperature of 30 ℃. Stirring uniformly, adding the cross-linking agent, stirring under vacuum degree of-0.1 MPa for 20min, subpackaging and discharging after the cross-linking agent is dispersed uniformly, and storing in a refrigerator. The storage temperature is generally controlled to be 2-8 ℃, and the storage period can be as long as 6 months. Samples were taken for curing and relevant tests were carried out, and the test results are shown in table one.
Example 2
The preparation method comprises the following steps:
(1) preparation of conductive filler and treating agent
Placing the conductive filler in a metal or ceramic disc, and baking for 2h in an oven at 50 ℃ to remove the moisture adsorbed in the conductive filler; and putting the conductive filler and the treating agent into a planetary stirrer according to the proportion of the conductive silica gel, and carrying out dispersion stirring for 20min at a stirring speed of 70rpm to obtain the conductive filler and the treating agent.
(2) Preparation of conductive silicon rubber material
Weighing various raw materials according to the proportion of the conductive silica gel, putting the two hydroxyl silicone oils with different viscosities, the MQ resin, the conductive filler, the treating agent and the filler into a planetary stirrer, stirring for 1.5h, dispersing rotating speed of 1250rpm, vacuum degree of-0.1 MPa and material temperature of 15 ℃. Stirring uniformly, adding the cross-linking agent, stirring under vacuum degree of-0.1 MPa for 10min, subpackaging and discharging after the cross-linking agent is dispersed uniformly, and storing in a refrigerator. The storage temperature is generally controlled to be 2-8 ℃, and the storage period can be as long as 6 months. Samples were taken for curing and relevant tests were carried out, and the test results are shown in table one.
Example 3
The preparation method comprises the following steps:
(1) preparation of conductive filler and treating agent
Placing the conductive filler in a metal or ceramic disc, and baking for 3h in an oven at 50 ℃ to remove the moisture adsorbed in the conductive filler; and putting the conductive filler and the treating agent into a planetary stirrer according to the proportion of the conductive silica gel, and carrying out dispersion stirring for 10min at a stirring speed of 40rpm to obtain the conductive filler and the treating agent.
(2) Preparation of conductive silicon rubber material
Weighing various raw materials according to the proportion of the conductive silica gel, firstly putting the two hydroxyl silicone oils with different viscosities, the MQ resin, the conductive filler, the treating agent and the filler into a planetary stirrer, stirring for 2 hours at a dispersion rotation speed of 2000rpm under a vacuum degree of-0.1 MPa and a material temperature of 10 ℃, adding the cross-linking agent after uniformly stirring, then stirring for 15 minutes under the vacuum degree of-0.1 MPa, subpackaging and discharging after the cross-linking agent is uniformly dispersed, and storing in a refrigerator. The storage temperature is generally controlled to be 2-8 ℃, and the storage period can be as long as 6 months. Samples were taken for curing and relevant tests were carried out, and the test results are shown in table one.
Watch 1
The main test methods of the product of the invention are as follows:
(1) time to surface dry
And (3) pointing the prepared single-component room-temperature vulcanized conductive adhesive into an adhesive tape with the height of 1mm and the length of 10mm by using a glue dispenser, and testing the time for which the surface is not sticky.
(2) Resistivity of
And (3) dispensing the prepared single-component room-temperature vulcanized conductive adhesive into an adhesive tape with the height of 1mm and the length of 10mm by using a dispenser, vulcanizing at room temperature for 24 hours, testing the resistance of the adhesive tape by using a low-resistance tester, and calculating the resistivity.
(3) Hardness of
The test is carried out according to GB/T531-1999 by a Shore durometer.
(4) Tensile strength and shear strength
Tensile strength was tested according to GB/T528-1998. The shear strength was measured according to GB/T7124-2008 tensile shear Strength of Adhesives (rigid Material to rigid Material) using aluminum sheets.
(5) Aging resistance test
And (3) pointing the prepared single-component room-temperature vulcanized conductive adhesive into an adhesive tape with the height of 1mm and the length of 10mm by using a dispensing device, ageing for 24 hours at 70 ℃ after 24-hour room-temperature vulcanization, testing the resistance of the single-component room-temperature vulcanized conductive adhesive by using a low-resistance tester, and calculating the change of the resistivity.
The conductive silica gel prepared by the invention has good conductive and shielding properties, the resistivity is about 0.01 omega cm, the hardness is moderate at 40-50 ℃, the mechanical strength is good, the adhesion is good, the shear strength with an aluminum sheet is more than 2.5MPa, the aging resistance is good, and the electrical property stability is good. Can meet the requirements of customers on the conductive silica gel.
Claims (4)
1. The single-component room temperature vulcanized conductive silica gel is characterized in that the conductive silica gel is prepared from the following raw materials in parts by weight:
silicon rubber-based rubber: a crosslinking agent: conductive filler and treating agent: filler = 100: 10-20: 300: 2-3;
wherein the weight ratio of the conductive filler to the treating agent is 100: 1-2;
the treating agent is prepared from the following raw materials in percentage by mass:
aminopropyltriethoxysilane: vinyltriethoxysilane = 2: 1;
the cross-linking agent is formed by mixing two raw materials of dichloromethyl triethoxysilane, diethylamino methyl triethoxysilane, aniline methyl triethoxysilane and aniline methyl trimethoxysilane;
the conductive filler is at least one of silver-plated copper powder, flake silver powder, nickel-plated graphite powder and conductive glass beads with the particle size of less than 50 micrometers;
the silicone rubber base glue is a combination of hydroxyl silicone oil and MQ resin, wherein the hydroxyl silicone oil is α, omega-dihydroxy polydimethylsiloxane, the viscosity is 1000-10000cp, and at the temperature of 25 ℃, the MQ resin is methyl MQ resin, and M is a monofunctional siloxane closed chain link (CH)3)3SiO1/2Q is tetrafunctional siloxane condensation mer SiO4/2M/Q is 0.8-1.0;
the preparation method of the single-component room temperature vulcanized conductive silica gel comprises the following steps:
step 1: preparation of conductive filler and treating agent
Placing the conductive filler in a metal or ceramic disc, and baking for 1-3 h in an oven at 50 ℃ to remove the water adsorbed in the conductive filler; putting the conductive filler and the treating agent into a planetary stirrer according to the proportion of the conductive silica gel, and carrying out dispersion stirring for 10-30 min at a stirring speed of 40-100 rpm to obtain the conductive filler and the treating agent;
step 2: preparation of conductive silicon rubber material
Weighing various raw materials according to the proportion of the conductive silica gel, firstly putting the silicone rubber base gel, the conductive filler, the treating agent and the filler into a planetary stirrer, stirring for 1-3 h at a dispersion rotation speed of 500-2000 rpm under a vacuum degree of-0.1 MPa and a material temperature of 10-30 ℃, adding the cross-linking agent after uniformly stirring, then stirring for 10-20 min under a vacuum degree of-0.1 MPa, subpackaging and discharging after the cross-linking agent is uniformly dispersed, and storing in a refrigerator.
2. The conductive silica gel of claim 1, wherein the filler is at least one of fumed silica, precipitated silica, and nano-sized titanium dioxide.
3. The conductive silica gel of claim 1, wherein the filler is a hydrophobic fumed silica surface-treated with dimethyldichlorosiloxane, and the specific surface area is 100 to 250m2/g。
4. A method for preparing the single-component room temperature vulcanized conductive silica gel of claim 1, comprising the following steps:
step 1: preparation of conductive filler and treating agent
Placing the conductive filler in a metal or ceramic disc, and baking for 1-3 h in an oven at 50 ℃ to remove the water adsorbed in the conductive filler; putting the conductive filler and the treating agent into a planetary stirrer according to the proportion of the conductive silica gel, and carrying out dispersion stirring for 10-30 min at a stirring speed of 40-100 rpm to obtain the conductive filler and the treating agent;
step 2: preparation of conductive silicon rubber material
Weighing various raw materials according to the proportion of the conductive silica gel, firstly putting the silicone rubber base gel, the conductive filler, the treating agent and the filler into a planetary stirrer, stirring for 1-3 h at a dispersion rotation speed of 500-2000 rpm under a vacuum degree of-0.1 MPa and a material temperature of 10-30 ℃, adding the cross-linking agent after uniformly stirring, then stirring for 10-20 min under a vacuum degree of-0.1 MPa, subpackaging and discharging after the cross-linking agent is uniformly dispersed, and storing in a refrigerator.
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| TWI632730B (en) * | 2016-11-29 | 2018-08-11 | 天邁科技股份有限公司 | Method of manufacturing waveguide assembly and structure thereof |
| CN107057367B (en) * | 2017-01-23 | 2020-12-08 | 青岛颐科密封材料有限公司 | Electromagnetic shielding sealing product and manufacturing process thereof |
| CN110358305B (en) * | 2019-07-10 | 2021-08-24 | 平湖阿莱德实业有限公司 | Nickel-plated powder filled elastomer with excellent weather resistance and preparation method thereof |
| CN115926469B (en) * | 2022-04-01 | 2023-10-13 | 徐州市中心医院 | Conductive silica gel plate and application thereof in nerve rehabilitation therapeutic apparatus |
| CN116082845A (en) * | 2023-01-05 | 2023-05-09 | 厦门牛转乾坤新材料有限公司 | Conductive silica gel and preparation method thereof |
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