CN108342055B - Fast-curing EMI heat-conducting and electric-conducting material and preparation method thereof - Google Patents
Fast-curing EMI heat-conducting and electric-conducting material and preparation method thereof Download PDFInfo
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- CN108342055B CN108342055B CN201810132867.0A CN201810132867A CN108342055B CN 108342055 B CN108342055 B CN 108342055B CN 201810132867 A CN201810132867 A CN 201810132867A CN 108342055 B CN108342055 B CN 108342055B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- 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
- C08K2003/085—Copper
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- 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
- C08K2003/0856—Iron
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- 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
Abstract
The invention belongs to the technical field of shielding materials, in particular to a fast-curing EMI heat-conducting and electric-conducting material and a preparation method thereof, which solve the problems of poor shielding effect, large difficulty in manufacturing process and low reproducibility existing in the prior art, and the fast-curing EMI heat-conducting and electric-conducting material comprises the following raw materials: bisphenol A epoxy resin, butadiene-styrene copolymer, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate, azodiisobutyronitrile, composite alloy powder and bisphenol A epoxy resin diluent; the preparation method comprises the following steps: s1, preparing composite alloy powder; s2, preparing raw materials of the EMI heat-conducting and electric-conducting material; s3, mixing the raw materials. The EMI heat-conducting and electricity-conducting material provided by the invention is simple in preparation method, convenient to use, short in curing time, good in shielding effect, excellent in heat-conducting and electricity-conducting properties and good in reproducibility.
Description
Technical Field
The invention relates to the technical field of shielding materials, in particular to a fast-curing EMI heat-conducting and electric-conducting material and a preparation method thereof.
Background
The principle of EMI, namely electromagnetic interference, is that electromagnetic energy transmission between a shielded area and the outside is blocked or attenuated by utilizing the reflection, absorption and guide effects of a shielding material on electromagnetic energy flow, and harmonic voltage and harmonic current formed between harmonic waves and the shielding material are led into the ground, so that the aim of shielding the harmonic waves is fulfilled. Common EMI shielding materials are mainly classified into four types: the composite material comprises conductive rubber, a conductive foam lining, a metal EMI lining, a conductive composite agent and a wave-absorbing material, wherein the conductive composite agent is widely applied to the fields of aerospace, automobiles, electronic devices, microwave equipment and the like due to the advantages of simple use method, wide application range, high shear strength, small thermal expansion coefficient, good heat and electricity conductivity and the like.
In recent years, more and more researchers have paid attention to the performance of EMI shielding materials, and chinese patent publication No. CN1653877A discloses a flame retardant, a conductive EMI shielding material and their manufacturing methods, in which the shielding material manufactured in the patent is composed of at least one layer of substance, which brings inconvenience to the manufacturing process of the shielding material, and the shielding material manufactured by the multi-layer structure has more influence factors on the shielding performance, which leads to poor production reproducibility of the shielding material, and the coating of the metal layer in the patent also brings great difficulty to the manufacturing process of the shielding material. Based on the defects in the prior art, the invention provides a fast-curing EMI heat-conducting and electric-conducting material and a preparation method thereof.
Disclosure of Invention
The invention aims to solve the defects of poor shielding effect, high difficulty in manufacturing process and low reproduction rate in the prior art, and provides a fast-curing EMI heat-conducting and electric-conducting material and a preparation method thereof.
A fast-curing EMI heat-conducting and electric-conducting material comprises the following raw materials in parts by weight: 60-80 parts of bisphenol A epoxy resin, 10-20 parts of butadiene-styrene copolymer, 0.2-0.6 part of trimethylolpropane, 1-1.5 parts of 4, 4' -diphenylmethane diisocyanate, 1-1.5 parts of xylene diisocyanate, 0.5-1.5 parts of dibutyltin dilaurate, 0.5-1.5 parts of azodiisobutyronitrile, 3-6 parts of composite alloy powder and 40-60 parts of bisphenol A epoxy resin diluent.
Preferably, the fast-curing EMI heat-conducting and electric-conducting material comprises the following raw materials in parts by weight: 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.2 parts of 4, 4' -diphenylmethane diisocyanate, 1.2 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azobisisobutyronitrile, 4 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent.
Preferably, the fast-curing EMI heat-conducting and electric-conducting material comprises the following raw materials in parts by weight: 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.3 parts of 4, 4' -diphenylmethane diisocyanate, 1.3 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azobisisobutyronitrile, 5 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent.
Preferably, the mass ratio of the bisphenol A epoxy resin to the butadiene-styrene copolymer is 4-6: 1.
preferably, the mass ratio of the 4, 4' -diphenylmethane diisocyanate to the xylene diisocyanate is 1: 1.
preferably, the composite alloy powder is prepared from the following components in a mass ratio of 1: 2-4, mixing copper powder and iron-based alloy powder, wherein the iron-based alloy powder comprises the following raw materials in percentage by weight: 2 to 4 percent of Co, 0.3 to 0.5 percent of Cr, 3 to 6 percent of Ni, 1 to 1.5 percent of Ag, 4 to 6 percent of Cu, 0.5 to 0.9 percent of Ge, 0.3 to 0.8 percent of Al, and the balance of Fe and inevitable impurities.
Preferably, the preparation method of the iron-based alloy powder comprises the following steps: adding raw materials of Co, Cr, Ni, Ag, Cu, Ge, Al and Fe into a smelting furnace, introducing inert gas into the smelting furnace, smelting, adding a DFC-800 type refining agent after the raw materials are completely molten, refining to obtain an iron-based alloy smelting liquid, and then introducing the iron-based alloy smelting liquid into an atomizer for atomization and powder preparation to obtain iron-based alloy powder.
Preferably, the flow rate of the iron-based alloy smelting liquid flowing into the atomizer is 16-18 kg/min, and the average particle size of the iron-based alloy powder after atomization powder preparation treatment is 40-60 microns.
The invention also provides a preparation method of the fast-curing EMI heat-conducting and electric-conducting material, which comprises the following steps:
s1, preparation of composite alloy powder: copper powder and iron-based alloy powder are mixed according to the mass ratio of 1: 2-4, adding the mixture into a ball mill, adding a grinding body with the mass being 2-3 times that of the mixture and ethanol with the mass being 0.5-1 time that of the mixture to perform ball milling and refining for 5-8 hours, and then drying the mixture to obtain composite alloy powder for later use;
s2, weighing the raw materials according to 60-80 parts of bisphenol A epoxy resin, 10-20 parts of butadiene-styrene copolymer, 0.2-0.6 part of trimethylolpropane, 1-1.5 parts of 4, 4' -diphenylmethane diisocyanate, 1-1.5 parts of xylene diisocyanate, 0.5-1.5 parts of dibutyltin dilaurate, 0.5-1.5 parts of azodiisobutyronitrile, 3-6 parts of composite alloy powder and 40-60 parts of bisphenol A epoxy resin diluent for later use;
and S3, mixing the bisphenol A epoxy resin weighed in the step S2 with a bisphenol A epoxy resin diluent at a stirring speed of 100-150 r/min, increasing the stirring speed to 150-180 r/min, adding the butadiene-styrene copolymer weighed in the step S2, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate and azodiisobutyronitrile in sequence after stirring is stable, increasing the stirring speed to 180-200 r/min after uniform mixing, adding the composite alloy powder weighed in the step S2, and stirring for 1-2 h to obtain the fast-curing EMI heat and electricity conducting material.
Preferably, the grinding body is a mixed steel ball with the diameter of 8-16 mm.
Compared with the prior art, the coating agent provided by the invention has the following technical effects:
1. the EMI heat-conducting and electricity-conducting material provided by the invention can be directly used, the curing time is short, the using method is simple, when in use, the EMI heat-conducting and electricity-conducting material is only needed to be coated and irradiated under an ultraviolet curing lamp for 1-2 min, the curing can be completed, and the coating after being cured into a film has excellent electric conduction and heat conduction performance and good shielding effect;
2. the EMI heat-conducting and electricity-conducting material is reasonable in formula, bisphenol A epoxy resin and butadiene-styrene copolymer are used as main materials, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate and azobisisobutyronitrile are added to enable the EMI heat-conducting and electricity-conducting material to have excellent curing performance, and then the EMI heat-conducting and electricity-conducting material is improved in shielding performance by being matched with composite alloy powder formed by mixing copper powder and iron-based alloy powder;
3. when the EMI heat and electricity conducting material is prepared, the composite alloy powder is subjected to ball milling and refining treatment so as to improve the granularity of the copper powder and the iron-based alloy powder and the mixing uniformity of the copper powder and the iron-based alloy powder, improve the distribution of the composite alloy powder in the EMI heat and electricity conducting material and further improve the consistency of the shielding performance of each part of the coating of the EMI heat and electricity conducting material after coating.
4. The EMI heat conduction material provided by the invention has the advantages of simple preparation method, good mixing uniformity of all raw materials, high reproducibility, easy development of the EMI heat conduction material during use, uniform and stable performance of a coating after use, and avoidance of difficulty in the preparation process due to the fact that the traditional EMI shielding material needs a multilayer structure.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example 1
The invention provides a fast-curing EMI heat-conducting and electric-conducting material which comprises the following raw materials in parts by weight: 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.2 parts of 4, 4' -diphenylmethane diisocyanate, 1.2 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azobisisobutyronitrile, 4 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent;
the preparation method comprises the following steps:
s1, preparation of composite alloy powder: copper powder and iron-based alloy powder are mixed according to the mass ratio of 1: 3, adding the mixture into a ball mill, adding a grinding body with the mass being 2 times that of the mixture and ethanol with the mass being 1 time that of the mixture, performing ball milling and refining for 6 hours, and then drying the mixture to obtain composite alloy powder for later use;
s2, weighing raw materials according to 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.2 parts of 4, 4' -diphenylmethane diisocyanate, 1.2 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azodiisobutyronitrile, 4 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent for later use;
s3, mixing the bisphenol A epoxy resin weighed in the step S2 with a bisphenol A epoxy resin diluent at a stirring speed of 120r/min, increasing the stirring speed to 160r/min, adding the butadiene-styrene copolymer weighed in the step S2, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate and azodiisobutyronitrile in sequence after stirring is stable, increasing the stirring speed to 190r/min after uniform mixing, adding the composite alloy powder weighed in the step S2, and stirring for 2h to obtain the fast-curing EMI heat and electricity conducting material.
In the invention, the iron-based alloy powder comprises the following raw materials in percentage by weight: 3% of Co, 0.4% of Cr, 5% of Ni, 1.2% of Ag1, 5% of Cu, 0.7% of Ge, 0.5% of Al and the balance of Fe and inevitable impurities; the preparation method of the iron-based alloy powder comprises the following steps: adding raw materials of Co, Cr, Ni, Ag, Cu, Ge, Al and Fe into a smelting furnace, introducing inert gas into the smelting furnace, smelting, adding a DFC-800 type refining agent after the raw materials are completely molten, refining to obtain an iron-based alloy smelting liquid, and then enabling the iron-based alloy smelting liquid to flow into an atomizer at a flow rate of 17kg/min for atomization and powder preparation to obtain iron-based alloy powder with the average particle size of 55 microns.
Example 2
The invention provides a fast-curing EMI heat-conducting and electric-conducting material which comprises the following raw materials in parts by weight: 80 parts of bisphenol A epoxy resin, 20 parts of butadiene-styrene copolymer, 0.6 part of trimethylolpropane, 1.5 parts of 4, 4' -diphenylmethane diisocyanate, 1.5 parts of xylene diisocyanate, 0.5 part of dibutyltin dilaurate, 0.5 part of azobisisobutyronitrile, 6 parts of composite alloy powder and 40 parts of bisphenol A epoxy resin diluent;
the preparation method comprises the following steps:
s1, preparation of composite alloy powder: copper powder and iron-based alloy powder are mixed according to the mass ratio of 1: 4, adding the mixture into a ball mill, adding a grinding body with the mass being 3 times that of the mixture and ethanol with the mass being 0.5 time that of the mixture for ball milling and refining for 5 hours, and then drying the mixture to obtain composite alloy powder for later use;
s2, weighing raw materials according to 80 parts of bisphenol A epoxy resin, 20 parts of butadiene-styrene copolymer, 0.6 part of trimethylolpropane, 1.5 parts of 4, 4' -diphenylmethane diisocyanate, 1.5 parts of xylene diisocyanate, 0.5 part of dibutyltin dilaurate, 0.5 part of azodiisobutyronitrile, 6 parts of composite alloy powder and 40 parts of bisphenol A epoxy resin diluent for later use;
s3, mixing the bisphenol A epoxy resin weighed in the step S2 with a bisphenol A epoxy resin diluent at a stirring speed of 150r/min, increasing the stirring speed to 180r/min, adding the butadiene-styrene copolymer weighed in the step S2, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate and azodiisobutyronitrile in sequence after stirring is stable, increasing the stirring speed to 200r/min after uniform mixing, adding the composite alloy powder weighed in the step S2, and stirring for 1h to obtain the fast-curing EMI heat and electricity conducting material.
In the invention, the iron-based alloy powder comprises the following raw materials in percentage by weight: 4% of Co, 0.5% of Cr, 3% of Ni, 1.5% of Ag1, 5% of Cu, 0.5% of Ge, 0.5% of Al and the balance of Fe and inevitable impurities; the preparation method of the iron-based alloy powder comprises the following steps: adding Co, Cr, Ni, Ag, Cu, Ge, Al and Fe raw materials into a smelting furnace, introducing inert gas into the smelting furnace, smelting, adding a DFC-800 type refining agent after the raw materials are completely molten, refining to obtain an iron-based alloy smelting liquid, and then enabling the iron-based alloy smelting liquid to flow into an atomizer at the flow rate of 18kg/min for atomization and powder preparation to obtain iron-based alloy powder with the average particle size of 40 microns.
Example 3
The invention provides a fast-curing EMI heat-conducting and electric-conducting material which comprises the following raw materials in parts by weight: 60 parts of bisphenol A epoxy resin, 10 parts of butadiene-styrene copolymer, 0.2 part of trimethylolpropane, 1 part of 4, 4' -diphenylmethane diisocyanate, 1 part of xylene diisocyanate, 1.5 parts of dibutyltin dilaurate, 1.5 parts of azobisisobutyronitrile, 3 parts of composite alloy powder and 60 parts of bisphenol A epoxy resin diluent;
the preparation method comprises the following steps:
s1, preparation of composite alloy powder: copper powder and iron-based alloy powder are mixed according to the mass ratio of 1: 2, adding the mixture into a ball mill, adding a grinding body with the mass being 2 times that of the mixture and ethanol with the mass being 1 time that of the mixture for ball milling and refining for 8 hours, and then drying the mixture to obtain composite alloy powder for later use;
s2, weighing the raw materials according to 60 parts of bisphenol A epoxy resin, 10 parts of butadiene-styrene copolymer, 0.2 part of trimethylolpropane, 1 part of 4, 4' -diphenylmethane diisocyanate, 1 part of xylene diisocyanate, 1.5 parts of dibutyltin dilaurate, 1.5 parts of azobisisobutyronitrile, 3 parts of composite alloy powder and 60 parts of bisphenol A epoxy resin diluent for later use;
s3, mixing the bisphenol A epoxy resin weighed in the step S2 with a bisphenol A epoxy resin diluent at a stirring speed of 100r/min, increasing the stirring speed to 150r/min, adding the butadiene-styrene copolymer weighed in the step S2, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate and azodiisobutyronitrile in sequence after stirring is stable, increasing the stirring speed to 180r/min after uniform mixing, adding the composite alloy powder weighed in the step S2, and stirring for 2h to obtain the fast-curing EMI heat and electricity conducting material.
In the invention, the iron-based alloy powder comprises the following raw materials in percentage by weight: co 2%, Cr 0.4%, Ni 6%, Ag 1%, Cu 6%, Ge 0.9%, Al 0.3%, and the balance Fe and inevitable impurities; the preparation method of the iron-based alloy powder comprises the following steps: adding raw materials of Co, Cr, Ni, Ag, Cu, Ge, Al and Fe into a smelting furnace, introducing inert gas into the smelting furnace, smelting, adding a DFC-800 type refining agent after the raw materials are completely molten, refining to obtain an iron-based alloy smelting liquid, and then enabling the iron-based alloy smelting liquid to flow into an atomizer at the flow rate of 16kg/min for atomization and powder preparation to obtain iron-based alloy powder with the average particle size of 60 microns.
Example 4
The invention provides a fast-curing EMI heat-conducting and electric-conducting material which comprises the following raw materials in parts by weight: 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.3 parts of 4, 4' -diphenylmethane diisocyanate, 1.3 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azobisisobutyronitrile, 5 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent;
the preparation method comprises the following steps:
s1, preparation of composite alloy powder: copper powder and iron-based alloy powder are mixed according to the mass ratio of 1: 3, adding the mixture into a ball mill, adding a grinding body with the mass being 3 times that of the mixture and ethanol with the mass being 0.5 time that of the mixture for ball milling and refining for 7 hours, and then drying the mixture to obtain composite alloy powder for later use;
s2, weighing raw materials according to 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.3 parts of 4, 4' -diphenylmethane diisocyanate, 1.3 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azodiisobutyronitrile, 5 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent for later use;
s3, mixing the bisphenol A epoxy resin weighed in the step S2 with a bisphenol A epoxy resin diluent at a stirring speed of 120r/min, increasing the stirring speed to 150r/min, adding the butadiene-styrene copolymer weighed in the step S2, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate and azodiisobutyronitrile in sequence after stirring is stable, increasing the stirring speed to 180r/min after uniform mixing, adding the composite alloy powder weighed in the step S2, and stirring for 2h to obtain the fast-curing EMI heat and electricity conducting material.
In the invention, the iron-based alloy powder comprises the following raw materials in percentage by weight: 3% of Co, 0.3% of Cr, 3% of Ni, 1.5% of Ag1, 4% of Cu, 0.5% of Ge, 0.8% of Al and the balance of Fe and inevitable impurities; the preparation method of the iron-based alloy powder comprises the following steps: adding Co, Cr, Ni, Ag, Cu, Ge, Al and Fe raw materials into a smelting furnace, introducing inert gas into the smelting furnace, smelting, adding a DFC-800 type refining agent after the raw materials are completely molten, refining to obtain an iron-based alloy smelting liquid, and then enabling the iron-based alloy smelting liquid to flow into an atomizer at the flow rate of 16-18 kg/min for atomization powder preparation treatment to obtain iron-based alloy powder with the average particle size of 50 microns.
Comparative example 1
The same mass of 4, 4' -diphenylmethane diisocyanate in example 1 was replaced with xylene diisocyanate under the same conditions as in example 1.
Comparative example 2
The same mass of xylene diisocyanate as in example 1 was replaced with 4, 4' -diphenylmethane diisocyanate under the same conditions as in example 1.
In the above examples 1, 2, 3, 4, 1 and 2, the grinding body is a mixed steel ball with a diameter of 8 to 16 mm.
Comparative example 3
The same mass of the composite alloy powder as in example 1 was replaced with silver powder, and the other conditions were the same as in example 1.
Experimental part:
1) testing of EMI thermal and electrical conductive materials:
the EMI thermal and electrical conductive materials prepared in example 1, example 2, example 3, example 4, comparative example 1 and comparative example 2 and the commercially available EMI shielding conductive adhesive TH6001 were used to perform a curing time test, respectively, and the curing time of the commercially available EMI shielding conductive adhesive TH6001 was used as a standard to measure other sets of experiments, and the results are shown in table 1.
Table 1:
in table 1, "-" indicates a value of a percentage of decrease in the test result value compared to the value of commercially available EMI shielding conductive paste TH 6001.
The results in table 1 show that the curing time of the EMI heat and electricity conductive material provided by the present invention is shortened by more than 19% compared with the curing time of commercially available EMI shielding and electricity conductive adhesive TH6001, which indicates that the curing time of the EMI heat and electricity conductive material provided by the present invention is short, and the curing time of the EMI heat and electricity conductive material can be significantly shortened by the combined use of 4, 4' -diphenylmethane diisocyanate and xylene diisocyanate.
2) The influence test of the composite alloy powder on the heat and electricity conducting performance of the EMI heat and electricity conducting material comprises the following steps:
the EMI conductive and thermal conductive materials prepared in example 1, example 2, example 3, example 4 and comparative example 3 were subjected to thermal conductivity and electrical conductivity tests, respectively, and the test results of example 1, example 2, example 3 and example 4 were evaluated as a standard against the test results of comparative example 3, and the results are shown in table 2.
Table 2:
the experimental results in table 2 show that the addition of the composite alloy powder in the formula of the EMI heat and electricity conductive material provided by the present invention can significantly improve the heat conductivity and the electricity conductivity of the EMI heat and electricity conductive material, and the heat conductivity and the electricity conductivity of the EMI heat and electricity conductive material prepared in examples 1 to 4 are significantly improved in heat conductivity and electricity conductivity compared to the EMI heat and electricity conductive material added with silver powder.
3) The reproducibility test of the preparation method of the EMI heat-conducting and electricity-conducting material provided by the invention
According to the formulation and preparation method of the EMI thermal and electrical conductive material of example 1, 6 batches of EMI thermal and electrical conductive materials were repeatedly prepared, and the electrical conductivity and the thermal conductivity of the 6 batches of EMI thermal and electrical conductive materials were tested, and the results are shown in table 3.
Table 3:
| test items | 1 | 2 | 3 | 4 | 5 | 6 |
| Thermal conductivity W/(m.K) | 8.5 | 8.4 | 8.6 | 8.3 | 8.5 | 8.4 |
| Conductivity S/cm | 7.3 | 7.3 | 7.5 | 7.2 | 7.4 | 7.2 |
The results in table 3 show that the formula and the preparation method of the EMI thermal and electrical conductive material provided by the present invention have good reproducibility, and 6 batches of EMI thermal and electrical conductive materials have small difference between thermal conductivity and electrical conductivity and good reproducibility.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. The fast-curing EMI heat-conducting and electric-conducting material is characterized by comprising the following raw materials in parts by weight: 60-80 parts of bisphenol A epoxy resin, 10-20 parts of butadiene-styrene copolymer, 0.2-0.6 part of trimethylolpropane, 1-1.5 parts of 4, 4' -diphenylmethane diisocyanate, 1-1.5 parts of xylene diisocyanate, 0.5-1.5 parts of dibutyltin dilaurate, 0.5-1.5 parts of azodiisobutyronitrile, 3-6 parts of composite alloy powder and 40-60 parts of bisphenol A epoxy resin diluent;
the composite alloy powder is prepared from the following components in percentage by mass of 1: 2-4, mixing copper powder and iron-based alloy powder, wherein the iron-based alloy powder comprises the following raw materials in percentage by weight: 2 to 4 percent of Co, 0.3 to 0.5 percent of Cr, 3 to 6 percent of Ni, 1 to 1.5 percent of Ag, 4 to 6 percent of Cu, 0.5 to 0.9 percent of Ge, 0.3 to 0.8 percent of Al, and the balance of Fe and inevitable impurities.
2. The fast-curing EMI thermal and electrical conductive material of claim 1, comprising the following raw materials in parts by weight: 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.2 parts of 4, 4' -diphenylmethane diisocyanate, 1.2 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azobisisobutyronitrile, 4 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent.
3. The fast-curing EMI thermal and electrical conductive material of claim 1, comprising the following raw materials in parts by weight: 70 parts of bisphenol A epoxy resin, 15 parts of butadiene-styrene copolymer, 0.4 part of trimethylolpropane, 1.3 parts of 4, 4' -diphenylmethane diisocyanate, 1.3 parts of xylene diisocyanate, 1 part of dibutyltin dilaurate, 1 part of azobisisobutyronitrile, 5 parts of composite alloy powder and 50 parts of bisphenol A epoxy resin diluent.
4. The fast-curing EMI thermal and electrical conducting material as claimed in claim 1, wherein the mass ratio of the bisphenol A epoxy resin to the butadiene-styrene copolymer is 4-6: 1.
5. the fast-curing EMI thermal and electrical conducting material according to claim 1, wherein the mass ratio of 4, 4' -diphenylmethane diisocyanate to xylylene diisocyanate is 1: 1.
6. the fast-curing EMI thermal and electrical conductive material of claim 1, wherein the preparation method of the iron-based alloy powder comprises the following steps: adding raw materials of Co, Cr, Ni, Ag, Cu, Ge, Al and Fe into a smelting furnace, introducing inert gas into the smelting furnace, smelting, adding a DFC-800 type refining agent after the raw materials are completely molten, refining to obtain an iron-based alloy smelting liquid, and then introducing the iron-based alloy smelting liquid into an atomizer for atomization and powder preparation to obtain iron-based alloy powder.
7. The fast-curing EMI thermal and electrical conduction material as claimed in claim 6, wherein the flow rate of the Fe-based alloy melt flowing into the atomizer is 16-18 kg/min, and the average particle size of the Fe-based alloy powder after the atomized powder processing is 40-60 μm.
8. The method of claim 1, comprising the steps of:
s1, preparation of composite alloy powder: copper powder and iron-based alloy powder are mixed according to the mass ratio of 1: 2-4, adding the mixture into a ball mill, adding a grinding body with the mass being 2-3 times that of the mixture and ethanol with the mass being 0.5-1 time that of the mixture to perform ball milling and refining for 5-8 hours, and then drying the mixture to obtain composite alloy powder for later use;
s2, weighing the raw materials according to 60-80 parts of bisphenol A epoxy resin, 10-20 parts of butadiene-styrene copolymer, 0.2-0.6 part of trimethylolpropane, 1-1.5 parts of 4, 4' -diphenylmethane diisocyanate, 1-1.5 parts of xylene diisocyanate, 0.5-1.5 parts of dibutyltin dilaurate, 0.5-1.5 parts of azodiisobutyronitrile, 3-6 parts of composite alloy powder and 40-60 parts of bisphenol A epoxy resin diluent for later use;
and S3, mixing the bisphenol A epoxy resin weighed in the step S2 with a bisphenol A epoxy resin diluent at a stirring speed of 100-150 r/min, increasing the stirring speed to 150-180 r/min, adding the butadiene-styrene copolymer weighed in the step S2, trimethylolpropane, 4' -diphenylmethane diisocyanate, xylene diisocyanate, dibutyltin dilaurate and azodiisobutyronitrile in sequence after stirring is stable, increasing the stirring speed to 180-200 r/min after uniform mixing, adding the composite alloy powder weighed in the step S2, and stirring for 1-2 h to obtain the fast-curing EMI heat and electricity conducting material.
9. The method for preparing the fast-curing EMI thermal and electrical conducting material as claimed in claim 8, wherein the grinding body is a mixed steel ball with a diameter of 8-16 mm.
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| US6221978B1 (en) * | 1998-04-09 | 2001-04-24 | Henkel Corporation | Moisture curable hot melt adhesive and method for bonding substrates using same |
| JP4114706B2 (en) * | 2005-02-18 | 2008-07-09 | 東洋インキ製造株式会社 | Electromagnetic wave shielding adhesive film, production method thereof, and electromagnetic wave shielding method for adherend |
| CN103571215A (en) * | 2012-07-18 | 2014-02-12 | 天瑞企业股份有限公司 | High thermal conductivity and EMI sheltering high polymer composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6221978B1 (en) * | 1998-04-09 | 2001-04-24 | Henkel Corporation | Moisture curable hot melt adhesive and method for bonding substrates using same |
| JP4114706B2 (en) * | 2005-02-18 | 2008-07-09 | 東洋インキ製造株式会社 | Electromagnetic wave shielding adhesive film, production method thereof, and electromagnetic wave shielding method for adherend |
| CN103571215A (en) * | 2012-07-18 | 2014-02-12 | 天瑞企业股份有限公司 | High thermal conductivity and EMI sheltering high polymer composite material |
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