CN113604192A - High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof - Google Patents
High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN113604192A CN113604192A CN202111010987.1A CN202111010987A CN113604192A CN 113604192 A CN113604192 A CN 113604192A CN 202111010987 A CN202111010987 A CN 202111010987A CN 113604192 A CN113604192 A CN 113604192A
- Authority
- CN
- China
- Prior art keywords
- parts
- nickel
- electromagnetic shielding
- silicone oil
- coated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000853 adhesive Substances 0.000 title claims abstract description 20
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 13
- 229910052710 silicon Inorganic materials 0.000 title claims description 13
- 239000010703 silicon Substances 0.000 title claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 88
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 40
- 239000004917 carbon fiber Substances 0.000 claims abstract description 40
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 40
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229920002545 silicone oil Polymers 0.000 claims abstract description 35
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 19
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000006229 carbon black Substances 0.000 claims abstract description 16
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000003112 inhibitor Substances 0.000 claims abstract description 5
- 239000004970 Chain extender Substances 0.000 claims abstract description 3
- 239000003085 diluting agent Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- 238000002791 soaking Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- -1 amino modified carbon Chemical class 0.000 claims description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 238000007747 plating Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- WVYQVVFYKDPKOS-UHFFFAOYSA-N [S].O.O.O.O.O.O.[Ni] Chemical compound [S].O.O.O.O.O.O.[Ni] WVYQVVFYKDPKOS-UHFFFAOYSA-N 0.000 claims description 7
- 239000011231 conductive filler Substances 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 7
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 claims description 4
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 4
- YFCGDEUVHLPRCZ-UHFFFAOYSA-N [dimethyl(trimethylsilyloxy)silyl]oxy-dimethyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C YFCGDEUVHLPRCZ-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 claims description 2
- COWFALGRNJAHKW-UHFFFAOYSA-N 3,6-dimethylhept-1-yn-3-ol Chemical compound CC(C)CCC(C)(O)C#C COWFALGRNJAHKW-UHFFFAOYSA-N 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 5
- DDCDEKHXBABHHI-UHFFFAOYSA-N acetylene cyclohexanol Chemical compound C1(CCCCC1)O.C#C DDCDEKHXBABHHI-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 238000004026 adhesive bonding Methods 0.000 abstract description 6
- 238000007789 sealing Methods 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 description 19
- 239000004594 Masterbatch (MB) Substances 0.000 description 14
- 239000011265 semifinished product Substances 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 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
-
- 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
- C09J11/08—Macromolecular additives
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
-
- 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
- C08K2201/001—Conductive additives
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-temperature addition type organosilicon electromagnetic shielding adhesive and a preparation method thereof, wherein the electromagnetic shielding adhesive comprises the following components in proportion: 400 parts of nickel-coated carbon fiber 200-100 parts of vinyl silicone oil, 5-20 parts of hydrogen-containing silicone oil, 30-80 parts of white carbon black, 0.5-2 parts of chain extender, 1-5 parts of tackifier, 0.1-0.3 part of inhibitor, 0.1-0.3 part of platinum catalyst and 10-30 parts of diluent. According to the invention, the nickel-coated carbon fiber is added into the system, so that the system can be reinforced, and good conductivity and electromagnetic shielding property are provided. After the spot gluing and curing, the volume resistance is less than 40m omega cm, the shielding effectiveness reaches more than 120dB, the tensile strength reaches 4.0MPa, the tearing strength is more than 20N/mm, the volume resistivity is only increased by about 12.5 percent of the initial volume resistivity after the spot gluing and curing, and the electromagnetic shielding effect can be kept to about 90 percent of the initial volume resistivity after the spot gluing and curing. The electromagnetic shielding adhesive has the characteristics of low cost, high conductivity, excellent mechanical property, good sealing property and stable electromagnetic shielding effect.
Description
Technical Field
The invention relates to the technical field of organic silicon viscose, in particular to a low-cost high-temperature addition type organic silicon electromagnetic shielding glue and a preparation method thereof.
Background
The electromagnetic shielding problem of electronic and electric appliances is always a great problem affecting the long-term stable use of electronic instruments and equipment. The electromagnetic shielding glue used by various electrical appliances at present mainly plays roles of bonding, sealing protection and electromagnetic shielding on components, wherein metal powder such as silver powder, copper powder and the like is usually mixed in the electromagnetic shielding glue for realizing the electromagnetic shielding effect, the price is expensive, other mechanical properties such as the sealing property, the bonding strength and the like of the electromagnetic shielding glue are gradually reduced along with the prolonging of time, the electromagnetic shielding effect is also reduced, the performance of electronic products is influenced, and the electromagnetic shielding glue can cause serious harm to human beings and other organisms. Therefore, there is a need in the related art for an electromagnetic shielding adhesive with low cost, high conductivity, excellent mechanical properties, good sealing performance, good electromagnetic shielding effect, and stability.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a low-cost high-temperature addition type organosilicon electromagnetic shielding glue and a preparation method thereof. The electromagnetic shielding glue has the characteristics of low cost, high conductivity, excellent mechanical property, good sealing property and stable electromagnetic shielding effect, and can solve the problems of unstable sealing property, bonding strength and electromagnetic shielding effect of the existing electromagnetic shielding glue.
The high-temperature addition type organic silicon electromagnetic shielding adhesive comprises the following components:
the conductive filler adopts nickel-coated carbon fiber, nickel-coated copper powder, nickel-coated silver powder, nickel-coated graphite powder, nickel powder, silver-coated copper powder or silver-coated aluminum powder to replace the traditional metal powder such as silver powder, copper powder and the like, and the electromagnetic shielding adhesive has the following components in preferred proportion: 400 parts of conductive filler 200, 80-100 parts of vinyl silicone oil, 5-20 parts of hydrogen-containing silicone oil, 30-80 parts of white carbon black, 0.5-2 parts of chain extender, 1-5 parts of tackifier, 0.1-0.3 part of inhibitor, 0.1-0.3 part of platinum catalyst and 10-30 parts of diluent. The above parts are all parts by weight, and the conductive filler can also adopt a combination of a plurality of different powders, wherein the nickel powder can be selected from one or a combination of a plurality of powders with the particle size of 50 μm, 100 μm and 150 μm in view of cost.
The vinyl silicone oil is preferably one or more of terminal vinyl silicone oil, side vinyl silicone oil and vinyl-terminated oligosiloxane.
The hydrogen-containing silicone oil is preferably one or two of hydrogen-containing silicone oil and end-side hydrogen silicone oil, and the viscosity of the hydrogen-containing silicone oil is 100-2000 mPas.
The white carbon black can be one or more of precipitation white carbon black, hydrophilic white carbon black and hydrophobic white carbon black.
The inhibitor is preferably one or more of 1-acetylene-1-cyclohexanol, 3-methyl-1-butyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol and 3, 6-dimethyl-1-heptyn-3-ol.
The solvent may be ethanol, acetone, kerosene, octamethyltrisiloxane, dimethyl carbonate, or decamethyltetrasiloxane.
The platinum content in the platinum catalyst is 3000-5000 ppm.
The preparation method of the high-temperature addition type organic silicon electromagnetic shielding glue comprises the following steps:
firstly, preparing nickel-coated carbon fibers:
(1) cutting the carbon fiber, washing with deionized water for many times, then soaking in 0.1mol/L coupling agent solution containing amino for 30-45min, heating at 110 ℃ for 30-45min, and repeating for many times to obtain the amino modified carbon fiber.
(2) Placing the amino modified carbon fiber in nickel sulfur hexahydrate (NiCl)2·6H2O) for 15-30min, and then adding sodium borohydride (NaBH)4) SolutionSoaking in the solution for 15-30min, and washing with deionized water for several times.
(3) And (3) putting the treated amino modified carbon fiber into a chemical nickel plating solution, reacting for 45-90min, repeatedly washing with deionized water for many times, and then putting into a 50 ℃ oven to bake for 45-90min to obtain the nickel-coated carbon fiber. The chemical nickel plating solution can adopt the following components:
and the other conductive fillers such as nickel-coated copper powder, nickel-coated silver powder, nickel-coated graphite powder, nickel powder, silver-coated copper powder or silver-coated aluminum powder and the like can be prepared by adopting the existing process or purchased directly on the market.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
The first embodiment is as follows:
step 1: 60 parts by weight of a vinyl silicone oil having a viscosity of 1 ten thousand, 40 parts by weight of a vinyl silicone oil having a viscosity of 2 ten thousand, 1.5 parts by weight of a silazane, and 0.5 part by weight of distilled water 1 were put into a kneader and stirred for 15 minutes. And adding 50 parts of fumed silica into the kneader in batches, stirring for 1 hour, heating to 150 ℃, and continuing stirring in vacuum for 3 hours to obtain a semi-finished product masterbatch.
Step 2:
(1) firstly, cutting 100 parts of carbon fiber by using a composite material cutting machine, washing the carbon fiber by using deionized water for 3 times, then soaking the carbon fiber in 0.1mol/L KH550 and other amino-containing coupling agent solutions for 20min, finally heating the carbon fiber at 110 ℃ for 20min, and repeating the steps for 3 times to obtain the amino-modified carbon fiber.
(2) Amino modified carbon fiber is added into nickel sulfur hexahydrate (NiCl)2·6H2O) for 15min, and then adding NaBH4Soaking in the solution for 15min, and washing with deionized water for 3 times.
(3) And (3) putting the treated amino modified carbon fiber into a chemical nickel plating solution, reacting for 15min, repeatedly washing for 3 times by using deionized water, and then putting into a 50 ℃ oven to bake for 30min to obtain the nickel-coated carbon fiber.
And step 3: taking 100 parts of the semi-finished product master batch, 10 parts of hydrogen-containing silicone oil with the average hydrogen content of 0.3%, 0.6 part of 4000ppm platinum catalyst, 0.06 part of 1-acetylene-1-cyclohexanol, 20 parts of nickel-coated carbon fiber, 180 parts of 50 mu m nickel powder and 20 parts of octamethyltrisiloxane, placing the mixture in a dispersion machine (the rotating speed is 100 revolutions per minute) and stirring the mixture for 10 minutes to prepare the high-temperature addition type organic silicon electromagnetic shielding adhesive.
Example two:
step 1: 60 parts of vinyl silicone oil having a viscosity of 1 ten thousand, 40 parts of vinyl silicone oil having a viscosity of 5 ten thousand, 1.5 parts of silazane and 0.5 part of distilled water 1 were added to a kneader and stirred for 15 minutes. And adding 40 parts of fumed silica into the kneader in batches, stirring for 1 hour, heating to 150 ℃, and continuing stirring in vacuum for 3 hours to obtain a semi-finished product masterbatch.
Step 2:
(1) firstly, cutting 100 parts of carbon fiber by using a composite material cutting machine, washing the carbon fiber by using deionized water for 3 times, then soaking the carbon fiber in 0.1mol/L KH550 and other amino-containing coupling agent solutions for 30min, finally heating the carbon fiber at 110 ℃ for 30min, and repeating the steps for 3 times to obtain the amino-modified carbon fiber.
(2) Putting amino modified carbon fiber into nickel sulfur hexahydrate (NiCl)2·6H2O) for 30min, and then adding NaBH4Soaking in the solution for 30min, and washing with deionized water for 3 times.
(3) And (3) putting the treated amino modified carbon fiber into a chemical nickel plating solution, reacting for 60min, repeatedly washing for 3 times by using deionized water, and then putting into a 50 ℃ oven to bake for 60min to obtain the nickel-coated carbon fiber.
And step 3: taking 100 parts of the semi-finished product master batch, 9 parts of hydrogen-containing silicone oil with the average hydrogen content of 0.61%, 0.5 part of 4000ppm platinum catalyst, 0.05 part of 3-methyl-1-butyne-3-ol, 30 parts of nickel-coated carbon fiber, 170 parts of 100 mu m nickel powder and 25 parts of decamethyltetrasiloxane, placing the mixture in a dispersion machine (the rotating speed is 100r), and stirring for 10min to prepare the high-temperature addition type organic silicon electromagnetic shielding adhesive.
Example three:
step 1: 100 parts of vinyl silicone oil having a viscosity of 1 ten thousand, 1.5 parts of silazane, and 0.5 part of distilled water were put into a kneader and stirred for 30 minutes. And adding 30 parts of white carbon black into the kneader in batches, stirring for 2 hours, heating to 150 ℃, and continuing to stir in vacuum for 3 hours to obtain a semi-finished product masterbatch.
Step 2:
(1) firstly, cutting 100 parts of carbon fiber by using a composite material cutting machine, washing with deionized water for 3 times, then soaking in 0.1mol/L KH550 and other amino-containing coupling agent solutions for 45min, finally heating at 110 ℃ for 45min, and repeating for 3 times to obtain the amino-modified carbon fiber.
(2) Putting amino modified carbon fiber into nickel sulfur hexahydrate (NiCl)2·6H2O) soaking for 30min, and adding NaBH4Soaking in the solution for 30min, and washing with deionized water for 3 times.
(3) And (3) putting the treated carbon fiber into a chemical nickel plating solution, reacting for 90min, repeatedly washing for 3 times by using deionized water, and then putting into a 50 ℃ oven to bake for 90min to obtain the nickel-coated carbon fiber.
And step 3: taking 100 parts of the semi-finished product master batch, 8 parts of hydrogen-containing silicone oil with average hydrogen content of 1.1%, 0.4 part of 4000ppm platinum catalyst, 0.04 part of 3, 5-dimethyl-1-hexyne-3-alcohol, 30 parts of nickel-coated carbon fiber, 170 parts of 100 mu m nickel powder and 30 parts of kerosene, placing the mixture in a dispersion machine (the rotating speed is 100r), and stirring for 10min to prepare the high-temperature addition type organic silicon electromagnetic shielding adhesive.
Example four:
step 1: 100 parts of vinyl silicone oil having a viscosity of 2 ten thousand, 1.5 parts of silazane, and 0.5 part of distilled water were put into a kneader and stirred for 30 minutes. And adding 30 parts of white carbon black into the kneader in batches, stirring for 2 hours, heating to 150 ℃, and continuing to stir in vacuum for 3 hours to obtain a semi-finished product masterbatch.
Step 2:
(1) firstly, cutting 100 parts of carbon fiber by using a composite material cutting machine, washing with deionized water for 3 times, then soaking in 0.1mol/L KH550 and other amino-containing coupling agent solutions for 45min, finally heating at 110 ℃ for 45min, and repeating for 3 times to obtain the amino-modified carbon fiber.
(2) Putting amino modified carbon fiber into nickel sulfur hexahydrate (NiCl)2·6H2O) soaking for 30min, and adding NaBH4Soaking in the solution for 30min, and washing with deionized water for 3 times.
(3) And (3) putting the treated carbon fiber into a chemical nickel plating solution, reacting for 90min, repeatedly washing for 3 times by using deionized water, and then putting into a 50 ℃ oven to bake for 90min to obtain the nickel-coated carbon fiber.
And step 3: taking 100 parts of the semi-finished product master batch, 7 parts of hydrogen-containing silicone oil with average hydrogen content of 1.1%, 0.4 part of 4000ppm platinum catalyst, 0.04 part of 3, 6-dimethyl-1-heptyne-3-alcohol, 30 parts of nickel-coated carbon fiber, 170 parts of 100 mu m nickel-coated silver powder and 30 parts of kerosene, and placing the mixture in a dispersion machine (the rotating speed is 100r) to stir for 10min to prepare the high-temperature addition type organic silicon electromagnetic shielding adhesive.
Example five:
step 1: 100 parts of vinyl silicone oil with the viscosity of 2 ten thousand, 1.5 parts of silazane and 0.5 part of distilled water are added into a kneader and stirred for 30 minutes; and adding 30 parts of white carbon black into the kneader in batches, stirring for 2 hours, heating to 150 ℃, and continuing to stir in vacuum for 3 hours to obtain a semi-finished product masterbatch.
Step 2:
(1) firstly, cutting 100 parts of carbon fiber by using a composite material cutting machine, washing with deionized water for 3 times, then soaking in 0.1mol/L KH550 and other amino-containing coupling agent solutions for 45min, finally heating at 110 ℃ for 45min, and repeating for 3 times to obtain the amino-modified carbon fiber.
(2) Amino modified carbon fiber is added into nickel sulfur hexahydrate (NiCl)2·6H2O) soaking for 30min, and adding NaBH4Soaking in the solution for 30min, and washing with deionized water for 3 times.
(3) And (3) putting the treated carbon fiber into a chemical nickel plating solution, reacting for 90min, repeatedly washing for 3 times by using deionized water, and then putting into a 50 ℃ oven to bake for 90min to obtain the nickel-coated carbon fiber.
And step 3: taking 100 parts of the semi-finished product master batch, 8 parts of hydrogen-containing silicone oil with average hydrogen content of 1.1%, 0.3 part of 4000ppm platinum catalyst, 0.04 part of 3, 5-dimethyl-1-hexyne-3-alcohol, 30 parts of nickel-coated carbon fiber, 170 parts of 100 mu m nickel-coated graphite powder and 30 parts of dimethyl carbonate, and placing the mixture in a dispersion machine (the rotating speed is 100r) to stir for 10min to prepare the high-temperature addition type organic silicon electromagnetic shielding adhesive.
Comparative example one:
step 1: 100 parts of vinyl silicone oil having a viscosity of 1 ten thousand, 1.5 parts of silazane, and 0.5 part of distilled water were added to a kneader and stirred for 30 minutes. And adding 30 parts of white carbon black into the kneader in batches, stirring for 2 hours, heating to 150 ℃, and continuing to stir in vacuum for 3 hours to obtain a semi-finished product masterbatch.
Step 2: 100 parts of the master batch, 8 parts of hydrogen-containing silicone oil with the average hydrogen content of 1.1 percent, 0.4 part of 3000ppm platinum catalyst, 0.04 part of 3-methyl-1-butyne-3-ol, 200 parts of 150 mu m nickel powder and 20 parts of acetone are put into a dispersion machine (the rotating speed is 100r) and stirred for 10min, and the organic silicon electromagnetic shielding adhesive for comparison is prepared.
Comparative example two:
step 1: 100 parts of vinyl silicone oil having a viscosity of 1 ten thousand, 1.5 parts of silazane, and 0.5 part of distilled water were added to a kneader and stirred for 30 minutes. And adding 30 parts of white carbon black into the kneader in batches, stirring for 2 hours, heating to 150 ℃, and continuing to stir in vacuum for 3 hours to obtain a semi-finished product masterbatch.
Step 2: 100 parts of the master batch, 8 parts of hydrogen-containing silicone oil with the average hydrogen content of 1.1%, 0.4 part of platinum catalyst with the average hydrogen content of 3000ppm, 0.04 part of 3-methyl-1-butyn-3-ol, 200 parts of 150 mu m nickel-coated graphite powder and 20 parts of octamethyltrisiloxane are put into a dispersion machine (the rotating speed is 100r) and stirred for 10min, and the organosilicon electromagnetic shielding adhesive for comparison is prepared.
The following table shows the data of the examples and comparative examples
As can be seen from the table, compared with the prior art, the invention has the advantage that the performance of each index is greatly improved.
The invention has the beneficial effects that: according to the invention, the nickel-coated carbon fiber is added into the system, so that the system can be reinforced, and good conductivity and electromagnetic shielding property are provided. After the spot gluing and curing, the volume resistance is less than 40m omega cm, the shielding effectiveness reaches more than 120dB, the tensile strength reaches 4.0MPa, the tearing strength is more than 20N/mm, the volume resistivity is only increased by about 12.5 percent of the initial volume resistivity after the spot gluing and curing, and the electromagnetic shielding effect can be kept to about 90 percent of the initial volume resistivity after the spot gluing and curing.
Claims (8)
1. The high-temperature addition type organosilicon electromagnetic shielding adhesive comprises a conductive filler and is characterized in that the conductive filler is one or a combination of more of nickel-coated carbon fiber, nickel-coated copper powder, nickel-coated silver powder, nickel-coated graphite powder, nickel powder, silver-coated copper powder and silver-coated aluminum powder.
2. The high-temperature addition type silicone electromagnetic shielding adhesive according to claim 1, comprising the following components: 200-400 parts of conductive filler, 80-100 parts of vinyl silicone oil, 5-20 parts of hydrogen-containing silicone oil, 30-80 parts of white carbon black, 0.5-2 parts of chain extender, 1-5 parts of tackifier, 0.1-0.3 part of inhibitor, 0.1-0.3 part of platinum catalyst and 10-30 parts of diluent.
3. The high temperature addition silicone electromagnetic shield glue of claim 2, wherein the vinyl silicone oil is a combination of one or more of a terminal vinyl silicone oil, a side vinyl silicone oil, a vinyl terminated oligosiloxane.
4. The high-temperature addition type silicone electromagnetic shielding adhesive according to claim 2, wherein the hydrogen-containing silicone oil is one of hydrogen-containing silicone oil, end side hydrogen silicone oil or a combination of two.
5. The high-temperature addition type organosilicon electromagnetic shielding adhesive according to claim 2, wherein the white carbon black is one or a combination of more of precipitated white carbon black, hydrophilic white carbon black and hydrophobic white carbon black.
6. The high temperature addition silicone electromagnetic shield gel of claim 2, wherein the inhibitor is one or a combination of more of 1-ethyne-1-cyclohexanol, 3-methyl-1-butyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3, 6-dimethyl-1-heptyn-3-ol.
7. The high temperature addition silicone electromagnetic shield according to claim 2, wherein the solvent is ethanol, acetone, kerosene, octamethyltrisiloxane, dimethyl carbonate, or decamethyltetrasiloxane.
8. A preparation method of a high-temperature addition type organic silicon electromagnetic shielding adhesive comprises the preparation of nickel-coated carbon fibers, and is characterized in that the preparation method of the nickel-coated carbon fibers comprises the following steps:
(1) cutting carbon fibers, washing the carbon fibers with deionized water for multiple times, then soaking the carbon fibers in 0.1mol/L of coupling agent solution containing amino for 30-45min, heating the carbon fibers at 110 ℃ for 30-45min, and repeating the steps for multiple times to obtain amino modified carbon fibers;
(2) placing the amino modified carbon fiber in nickel sulfur hexahydrate (NiCl)2·6H2O) for 15-30min, and then adding NaBH4Soaking in the solution for 15-30min, and washing with deionized water for multiple times;
(3) and (3) putting the treated amino modified carbon fiber into a chemical nickel plating solution, reacting for 45-90min, repeatedly washing with deionized water for many times, and then putting into a 50 ℃ oven to bake for 45-90min to obtain the nickel-coated carbon fiber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111010987.1A CN113604192A (en) | 2021-08-31 | 2021-08-31 | High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111010987.1A CN113604192A (en) | 2021-08-31 | 2021-08-31 | High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113604192A true CN113604192A (en) | 2021-11-05 |
Family
ID=78342328
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111010987.1A Pending CN113604192A (en) | 2021-08-31 | 2021-08-31 | High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113604192A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115109562A (en) * | 2022-08-09 | 2022-09-27 | 广州市白云化工实业有限公司 | Bi-component high-heat-dissipation high-conductivity organic silicon pouring sealant and preparation method thereof |
| CN115873556A (en) * | 2022-12-23 | 2023-03-31 | 广州市白云化工实业有限公司 | High-resilience electromagnetic shielding adhesive and preparation method thereof |
| CN115926737A (en) * | 2022-12-06 | 2023-04-07 | 锐腾新材料制造(苏州)有限公司 | Electromagnetic shielding adhesive convenient for heat conduction and heat dissipation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005194372A (en) * | 2004-01-07 | 2005-07-21 | Shin Etsu Polymer Co Ltd | Silicone adhesive |
| CN102276988A (en) * | 2011-06-08 | 2011-12-14 | 北京工业大学 | Mono-component Ni-C filled-type FIP (Form In Place) heat-curing highly-conductive silicone rubber and preparation method thereof |
| CN102644069A (en) * | 2012-05-22 | 2012-08-22 | 东北林业大学 | Method for chemically plating nickel on surface of carbon fiber |
-
2021
- 2021-08-31 CN CN202111010987.1A patent/CN113604192A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005194372A (en) * | 2004-01-07 | 2005-07-21 | Shin Etsu Polymer Co Ltd | Silicone adhesive |
| CN102276988A (en) * | 2011-06-08 | 2011-12-14 | 北京工业大学 | Mono-component Ni-C filled-type FIP (Form In Place) heat-curing highly-conductive silicone rubber and preparation method thereof |
| CN102644069A (en) * | 2012-05-22 | 2012-08-22 | 东北林业大学 | Method for chemically plating nickel on surface of carbon fiber |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115109562A (en) * | 2022-08-09 | 2022-09-27 | 广州市白云化工实业有限公司 | Bi-component high-heat-dissipation high-conductivity organic silicon pouring sealant and preparation method thereof |
| CN115109562B (en) * | 2022-08-09 | 2024-03-12 | 广州白云科技股份有限公司 | Double-component high-heat-dissipation high-conductivity organic silicon pouring sealant and preparation method thereof |
| CN115926737A (en) * | 2022-12-06 | 2023-04-07 | 锐腾新材料制造(苏州)有限公司 | Electromagnetic shielding adhesive convenient for heat conduction and heat dissipation |
| CN115873556A (en) * | 2022-12-23 | 2023-03-31 | 广州市白云化工实业有限公司 | High-resilience electromagnetic shielding adhesive and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113604192A (en) | High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof | |
| CN106467668B (en) | Organic silicon resin aluminum-based copper-clad plate and preparation method thereof | |
| CN101654605B (en) | Modified epoxy resin adhesive and preparation method thereof | |
| CN109370235B (en) | Double-component addition type organic silicon gel and preparation method thereof | |
| CN104312476A (en) | Silver coated copper powder conductive adhesive and preparation method thereof | |
| KR100808146B1 (en) | Compositions of thin conductive tape for EMI shielding, method thereof and products manufactured therefrom | |
| CN110564107B (en) | Efficient electromagnetic shielding composite material and preparation method thereof | |
| KR20180099832A (en) | Electro-conductive curable organosilicon rubber | |
| CN112646377A (en) | Conductive silicone rubber for electromagnetic shielding and preparation method thereof | |
| CN110922762A (en) | High-conductivity silica gel composition based on conductive powder wet modification technology | |
| CN113105862A (en) | Preparation method of heat-resistant organic silicon pressure-sensitive adhesive | |
| CN110093130A (en) | A kind of electromagnetic shielding conductive silver glue and preparation method thereof | |
| CN113990557A (en) | Preparation method and application of elastomer with high conductivity and high stretchability | |
| CN114605834A (en) | High-conductivity rubber material with electromagnetic shielding function and manufacturing method thereof | |
| CN110845851B (en) | Liquid conductive adhesive for power cable accessories and preparation method thereof | |
| CN115011294B (en) | Sintered nano silver conductive adhesive for chip packaging and preparation method thereof | |
| CN114517053A (en) | High-hydrophobicity anti-pollution flashover coating and preparation method thereof | |
| CN116285219A (en) | Epoxy resin composite material with excellent tracking resistance, preparation method and application thereof | |
| CN116082580A (en) | Powder surface modifier, modified powder and preparation method and application thereof | |
| CN103059570A (en) | Conductive rubber | |
| CN113956838A (en) | Radiation modified electromagnetic shielding silicone rubber self-adhesive tape and preparation method thereof | |
| CN113416481A (en) | Electromagnetic wave shielding composite coating and preparation method thereof | |
| CN111978908A (en) | Low-viscosity high-heat-conductivity pouring sealant | |
| KR20170102230A (en) | Conductive paste | |
| CN112521751B (en) | Silicon resin composition and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211105 |
|
| RJ01 | Rejection of invention patent application after publication |