CN106954380B - Multi-loss mechanism wave-absorbing shielding material and preparation method thereof - Google Patents
Multi-loss mechanism wave-absorbing shielding material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a multi-loss mechanism wave-absorbing shielding material which is composed of magnetic medium type wave-absorbing shielding material nickel/cobalt nano particles, resistance type wave-absorbing shielding material silicon carbide fibers, perovskite type high dielectric loss wave-absorbing shielding material and an overflow-seepage structure composite resistance type wave-absorbing shielding material formed by Reduced Graphene Oxide (RGO) and polyphenylene sulfide (PPS). The invention also provides a preparation method of the multi-loss mechanism wave-absorbing shielding material. The multi-loss mechanism wave-absorbing shielding material has the advantages of customized design, can meet the structural requirements, design requirements, process requirements, use environment requirements and the like of different parts by adjusting the proportion of a formula, has the characteristics of high absorption peak value, wide frequency band, low density and the like, conforms to the development trend of 'high, thin, light and wide' of the current wave-absorbing shielding material, can be applied to various fields, and has wide industrial application prospect.
Description
Technical Field
The invention provides a multi-loss mechanism wave-absorbing shielding material and a preparation method thereof, belonging to the field of wave-absorbing shielding materials.
Background
The wave-absorbing material is a functional material which can absorb and attenuate the electromagnetic wave energy projected to the surface of the wave-absorbing material, and convert the electromagnetic wave energy into heat energy or dissipate other energy through dielectric loss, resistance loss, magnetic loss and the like of the material, or eliminate the electromagnetic wave due to interference, so that the reflection, the scattering and the transmission are very small. The electromagnetic wave processing principle is divided into absorption mode and interference extinction mode.
The electromagnetic wave shielding material generally refers to a material capable of shielding a certain space region from other devices and ensuring that the space is not interfered by the outside. The electromagnetic wave processing principle is classified into a reflection type and an absorption type. Most of the traditional electromagnetic shielding materials are reflective, the single-function reflected electromagnetic waves only can ensure the electromagnetic environment in a shielding area, the energy of the interfering electromagnetic waves is basically not attenuated after being reflected, and more electromagnetic interference and harm are caused along with the superposition of the reflection times in a relatively closed area. Not to mention the additional problems of the reflective shielding material to the manufacturing process, such as the high process tolerance required by the necessary shielding tape winding section in the cable process, and the design limitations of the shielding of electronic precision parts and shaped parts, which are often difficult for the material and engineering designer.
The scheme of the wave-absorbing shielding material can solve various problems and defects brought by the traditional reflection-type electromagnetic shielding, and the wave-absorbing shielding material development currently presents the following development trend: 1. the density is reduced; 2. compounding; 3. performing multi-spectrum compatibility; 4. intelligence, etc. The wave-absorbing shielding material with a multi-loss mechanism becomes one of the optimal solutions in compliance with the development. The customizable multi-loss mechanism wave-absorbing shielding material is a composite wave-absorbing shielding material system with various loss type wave-absorbing shielding materials, can be subjected to customized formula design, customized structure design, customized process design and the like according to various factors such as different part structure requirements, design requirements, use environments and the like, and is also a hotspot for the development of the conventional wave-absorbing shielding materials. The customizable multi-loss mechanism wave-absorbing shielding material generally consists of various different loss types of wave-absorbing shielding materials and a base material, and the selection and the proportion of the wave-absorbing shielding materials are often determined by factors such as preset application environment, frequency, bandwidth and the like. At the same time, the choice of the matrix material is also important, since it must take into account the following 2 items: firstly, the compatibility problem of the matrix material and different wave-absorbing shielding materials (mainly inorganic materials), namely the interface stability problem of the composite material, and secondly, the dispersion uniformity problem during mixing can influence various quality indexes of the finished product.
The multi-loss mechanism wave-absorbing shielding material provided by the invention specifically comprises the following components: 1. magnetic medium type wave-absorbing shielding material nickel/cobalt nano-particles; 2. resistance type wave-absorbing shielding material silicon carbide fiber; 3. perovskite dielectric wave-absorbing shielding materials; 4. the graphene and the polyphenylene sulfide form a composite resistance type wave-absorbing shielding material with an overflow-seepage network structure.
Disclosure of Invention
One purpose of the invention is to provide a formula of a multi-loss mechanism wave-absorbing shielding material; the invention also aims to provide a preparation method of the multi-loss mechanism wave-absorbing shielding material.
A multi-loss mechanism wave-absorbing shielding material is composed of magnetic medium type wave-absorbing shielding material nickel/cobalt nanoparticles, resistance type wave-absorbing shielding material silicon carbide fibers, perovskite type high dielectric loss type wave-absorbing shielding materials, and an overflow-seepage structure composite resistance type wave-absorbing shielding material formed by Reduced Graphene Oxide (RGO) and polyphenylene sulfide (PPS).
The nickel/cobalt nanoparticles, the silicon carbide fiber, the perovskite material and the Reduced Graphene Oxide (RGO) are 1-40: 1-10: 40-80 in molar ratio.
The number of segments of polyphenylene sulfide (PPS) is preferably 2-4 times the sum of the amounts of nickel/cobalt nanoparticles, silicon carbide fibers, perovskite-type materials and Reduced Graphene Oxide (RGO) substances.
The perovskite high dielectric loss type wave-absorbing shielding material is any one of barium titanate (BaTiO3), calcium titanate (CaTiO3) or strontium titanate (SrTiO 3).
The polyphenylene sulfide (PPS) is not limited to the number of segments of polyphenylene sulfide, i.e., weight average molecular weight per molecular weight of the structural unit, which is arbitrarily taken herein, but is assumed to have a molecular weight of 109.17, for the purpose of determining the amount of 1, 4-p-dichlorobenzene which is a reactant.
A preparation method of a multi-loss mechanism wave-absorbing shielding material comprises the following steps:
and S1, mixing and dispersing the precursors.
Putting the corresponding nickel/cobalt nano precursor (nickel chloride/cobalt chloride) in the step 1, silicon carbide fiber, perovskite, Reduced Graphene Oxide (RGO) precursor Graphene Oxide (GO), 1, 4-p-dichlorobenzene, sulfide, sodium phosphate and the like into an organic solvent system, and ultrasonically dispersing for 15-20 min for later use.
The sulfide is preferably sodium sulfide or potassium sulfide.
The amount of the 1, 4-p-dichlorobenzene is equal to the number of the polyphenylene sulfide segments in the 1, 4-p-dichlorobenzene, sulfide, sodium phosphate and an organic solvent system in a molar ratio of 1: 2-3: 0.001-0.01: 2-3.
The organic solvent system consists of N-methylpyrrolidone (NMP), Dimethylformamide (DMF) and hexamethylphosphoric triamide (HMPA), and the mol ratio of N-methylpyrrolidone (NMP) to Dimethylformamide (DMF) to hexamethylphosphoric triamide (HMPA) is preferably 45: 10.
S2, respectively injection molding the multi-loss mechanism wave-absorbing shielding material into test pieces with corresponding test requirementsPost-processivity
Can be tested.
S3, the dielectric property, the magnetic property and the wave-absorbing property of the multi-loss mechanism wave-absorbing shielding material are that the finished product is injected and molded Polishing and cleaning the test piece of the photo holder, and processing the test piece by Agilent-N5230AModel (III)Network vector analyzer analysis The frequency is 2-18 GHz.
S4, reducing graphene oxide, reducing nickel chloride/cobalt chloride to generate polyphenylene sulfide (PPS) prepolymer, and polycondensing the polyphenylene sulfide (PPS).
Dissolving sodium hydroxide into hydrazine hydrate to prepare a solution, dropwise adding the solution into the standby dispersion liquid obtained in the step A, wherein the molar ratio of nickel chloride to cobalt chloride to sodium hydroxide to hydrazine hydrate is 0.5: 13-15: 32-40, then placing the dispersion liquid into a reaction kettle, reacting for 3-5 h at the temperature of 150-220 ℃ and the pressure of 0.02-0.04 MPa, reacting for 2-3 h at the temperature of 230-280 ℃ and the pressure of 0.3-0.6 MPa, carrying out suction filtration, then placing filter residues into an extruder for granulation, and finally forming the product, namely the customized multi-loss mechanism wave-absorbing shielding material.
Compared with the prior art, the customizable multi-loss mechanism wave-absorbing shielding material has the following advantages:
1. the product of the invention comprises magnetic medium type wave-absorbing shielding material nickel/cobalt nano particles, resistance type wave-absorbing shielding material silicon carbide fiber, dielectric medium type wave-absorbing shielding material perovskite, and composite resistance type wave-absorbing shielding material with an overflow-seepage network structure consisting of graphene and polyphenylene sulfide.
2. The customized design has advantages, and different product structure requirements, design requirements, process requirements, use environment requirements and the like can be met by adjusting the proportion of the formula.
3. Complementary optimization of multi-mechanism action reserves enough flexibility for the next step structure, and does not cause the situation that the material design usually has the disadvantage of considering the same.
4. The multi-loss mechanism wave-absorbing shielding material has the characteristics of high absorption peak value, wide frequency band, low density and the like, and conforms to the development trend of 'high, thin, light and wide' of the current wave-absorbing shielding material;
5. the method has the advantages of relatively simple process, good tolerance, good secondary processing performance of products and wide application field, can be applied to various fields such as electromagnetic compatibility (EMC) and electromagnetic interference (EMI) electronic components, electromagnetic radiation protection of mobile phones and computers, electromagnetic radiation protection of broadcasting and television transmitting stations, electromagnetic radiation protection of industrial, scientific and medical equipment, electromagnetic radiation protection of buildings in offices and residential areas, electromagnetic radiation protection required by household appliances and the like, and has wide industrial application prospect.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, technical solutions of exemplary embodiments of the present invention will be further described below. Unless otherwise specified, all reagents used in the examples are commercially available reagents, and all procedures used are routine in the art.
Example 1
And S1, mixing and dispersing the precursors.
Putting nickel chloride/cobalt chloride, silicon carbide fiber, perovskite, Graphene Oxide (GO), 1, 4-p-dichlorobenzene, sodium sulfide, sodium phosphate and the like into an organic solvent system, and ultrasonically dispersing for 15-20 min for later use.
2mol of nickel chloride, 2mol of silicon carbide fiber, 0.5mol of calcium titanate and 6mol of Graphene Oxide (GO) are selected.
Let the number of segments of polyphenylene sulfide be equal to 3 times the sum of the amounts of nickel chloride, silicon carbide fiber, calcium titanate, and graphene oxide (RGO) substances.
Selecting 31.5mol of 1, 4-p-dichlorobenzene, 78.75mol of sodium sulfide, 0.1575mol of sodium phosphate and 78.75mol of organic solvent system.
The solvent system comprises N-methyl pyrrolidone, dimethyl formamide, hexamethyl phosphoric triamide (45: 10) according to molar ratio.
S2, respectively injection molding the multi-loss mechanism wave-absorbing shielding material into test pieces with corresponding test requirements, and performing progressive test
Can be tested.
S3, the dielectric property, the magnetic property and the wave-absorbing property of the multi-loss mechanism wave-absorbing shielding material are that the finished product is injected and molded
Forming corresponding test piece, polishing, cleaning, and separating with Agilent-N5230A type network vector analyzerAnalysis and measurement
The frequency is 2-18 GHz.
S4, reducing graphene oxide, reducing nickel chloride/cobalt chloride to generate polyphenylene sulfide (PPS) prepolymer, and polycondensing the polyphenylene sulfide (PPS).
Dissolving sodium hydroxide into hydrazine hydrate to prepare a solution, dropwise adding the solution into the standby dispersion liquid obtained in the step A, then putting the dispersion liquid into a reaction kettle, reacting for 4 hours at 200 ℃ and 0.03MPa, reacting for 2.5 hours at 260 ℃ and 0.5MPa, carrying out suction filtration, putting filter residues into an extruder for granulation, and finally forming the product, namely the customized multi-loss mechanism wave-absorbing shielding material.
56mol of sodium hydroxide and 144mol of hydrazine hydrate are selected.
Examples 2 to 9
In the embodiments 2 to 9, the proportion of nickel chloride, silicon carbide fiber, calcium titanate and Graphene Oxide (GO) is changed, and the corresponding 1, 4-p-dichlorobenzene and the like are also changed, so as to investigate the performance of the wave-absorbing shielding material controlled by the change of the proportion. See Table below ("-" represents the same as example 1)
Examples 10 to 11
In examples 10 to 11, the number of segments of the polyphenylene sulfide produced was changed, and in example 10, the number of segments of the polyphenylene sulfide was set to be 2 times the sum of the amounts of nickel chloride, silicon carbide fiber, calcium titanate, and Graphene Oxide (GO), and accordingly, 21mol of 1, 4-p-dichlorobenzene, 52.5mol of sodium sulfide, 0.105mol of sodium phosphate, and 52.5mol of an organic solvent system were used. In example 11, it is assumed that the number of segments of polyphenylene sulfide is 4 times the sum of the amounts of nickel chloride, silicon carbide fiber, calcium titanate, and Graphene Oxide (GO), and that 42mol of 1, 4-p-dichlorobenzene, 105mol of sodium sulfide, 0.21mol of sodium phosphate, and 105mol of organic solvent system are involved. The remaining parameters not mentioned are the same as in example 1.
Examples 12 to 13
In the embodiments 12-13, the perovskite high dielectric loss type wave-absorbing shielding material is changed, barium titanate is adopted in the embodiment 12, and strontium titanate is adopted in the embodiment 13. The remaining parameters not mentioned are the same as in example 1.
Example 14
Example 14 modification of sulfide to Potassium sulfide, the remaining parameters not mentioned being identical to those of example 1
Examples 15 to 20
In examples 15 to 20, the reaction conditions of polyphenylene sulfide formation were examined by changing the amounts of sodium sulfide, sodium phosphate and organic solvent system substances, respectively. See table below ("-" represents the same as example 1), the remaining parameters not mentioned are the same as example 1.
Examples 21 to 24
In examples 21 to 24, the amounts of sodium hydroxide and hydrazine hydrate were varied, and reduction of nickel chloride and graphene was examined. See table below ("-" represents the same as example 1), the remaining parameters not mentioned are the same as example 1.
Performance testing
The multi-loss mechanism wave-absorbing shielding material prepared in the embodiment 1 to 24 is injected into a test piece with corresponding test requirements, and then the performance test is carried out. The test items and methods were as follows:
1. wave-absorbing property, dielectric property and magnetic property
The dielectric property, the magnetic property and the wave-absorbing property of the prepared multi-loss mechanism wave-absorbing shielding material are that a finished product is injected into a corresponding test piece (a wafer or a ring piece), the test piece is subjected to polishing and cleaning treatment and is analyzed and tested by an Agilent-N5230A type network vector analyzer, and the frequency is 2-18 GHz.
2. Volume resistivity
The test is carried out according to the national standard GB/T1410-2006.
3. Heat distortion temperature
According to the national standard GB/T1633-2000, the heat distortion Vicat temperature is measured by adopting a FYWK-300 heat distortion Vicat temperature measuring instrument.
4. Tensile strength
The test is carried out according to the national standard GB/T1040-.
The test results are given in the following table:
and (3) performance test results:
Claims (2)
1. a multi-loss mechanism wave-absorbing shielding material is characterized in that: the composite resistance type wave-absorbing shielding material consists of magnetic medium type wave-absorbing shielding material nickel/cobalt nano particles, resistance type wave-absorbing shielding material silicon carbide fibers, perovskite type high dielectric loss type wave-absorbing shielding material, and an overflow-seepage structure composite resistance type wave-absorbing shielding material formed by Reduced Graphene Oxide (RGO) and polyphenylene sulfide (PPS);
the nickel/cobalt nanoparticles, the silicon carbide fibers, the perovskite material and the Reduced Graphene Oxide (RGO) are 1-40: 1-10: 40-80 in molar ratio;
the perovskite high dielectric loss type wave-absorbing shielding material is any one of barium titanate (BaTiO3), calcium titanate (CaTiO3) or strontium titanate (SrTiO 3);
the number of segments of the polyphenylene sulfide (PPS) is 2-4 times of the sum of the amounts of nickel/cobalt nanoparticles, silicon carbide fibers, perovskite materials and Reduced Graphene Oxide (RGO) substances, the amount of the reactant 1, 4-dichlorobenzene is determined, the number of segments of the polyphenylene sulfide is the weight average molecular weight/the molecular weight of a structural unit, the weight average molecular weight is arbitrarily selected, and the molecular weight of the structural unit is 109.17.
2. The method for preparing the multi-loss mechanism wave-absorbing shielding material according to claim 1, wherein the method comprises the following steps: comprises the following steps of (a) carrying out,
s1, mixing and dispersing the precursor;
putting the nickel/cobalt nano precursor of nickel/cobalt chloride, silicon carbide fiber, perovskite, Reduced Graphene Oxide (RGO) precursor Graphene Oxide (GO), 1, 4-p-dichlorobenzene, sulfide and sodium phosphate in an organic solvent system, and ultrasonically dispersing for 15-20 min for later use;
the sulfide is sodium sulfide or potassium sulfide;
the amount of the 1, 4-p-dichlorobenzene is equal to the number of the polyphenylene sulfide segments in claim 1, and the molar ratio of the 1, 4-p-dichlorobenzene to the sulfide to the sodium phosphate to the organic solvent system is 1: 2-3: 0.001-0.01: 2-3;
the organic solvent system consists of N-methylpyrrolidone (NMP), Dimethylformamide (DMF) and hexamethylphosphoric triamide (HMPA), and the molar ratio of the N-methylpyrrolidone (NMP) to the Dimethylformamide (DMF) to the hexamethylphosphoric triamide (HMPA) is 45: 10;
s2, reducing graphene oxide, reducing nickel chloride/cobalt chloride to generate a polyphenylene sulfide (PPS) prepolymer, and polycondensing the polyphenylene sulfide (PPS);
dissolving sodium hydroxide into hydrazine hydrate to prepare a solution, dropwise adding the solution into the standby dispersion liquid obtained in the step A, then putting the dispersion liquid into a reaction kettle, reacting for 3-5 h at the temperature of 150-220 ℃ and the pressure of 0.02-0.04 MPa, reacting for 2-3 h at the temperature of 230-280 ℃ and the pressure of 0.3-0.6 MPa, carrying out suction filtration, putting filter residues into an extruder for granulation, and finally forming the product, namely the customized multi-loss mechanism wave-absorbing shielding material;
the molar ratio satisfies the condition that the ratio of nickel chloride/cobalt chloride, sodium hydroxide and hydrazine hydrate is 0.5: 13-15: 32-40;
s3, respectively injection-molding the multi-loss mechanism wave-absorbing shielding material into test pieces with corresponding test requirements, and then carrying out performance test;
s4, the dielectric property, the magnetic property and the wave-absorbing property of the multi-loss mechanism wave-absorbing shielding material are that a finished product is injection-molded into a corresponding test piece, and the test piece is subjected to polishing and cleaning treatment and is analyzed and tested by an Agilent-N5230A type network vector analyzer, wherein the frequency is 2-18 GHz.
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| CN110105761A (en) * | 2019-05-20 | 2019-08-09 | 四川大学 | Graphene/polyphenylene sulfide electromagnetic shielding composite material and preparation method thereof |
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