CN114874609B - High-damping intelligent vibration-damping sheet material and preparation method thereof - Google Patents

High-damping intelligent vibration-damping sheet material and preparation method thereof Download PDF

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CN114874609B
CN114874609B CN202210214570.5A CN202210214570A CN114874609B CN 114874609 B CN114874609 B CN 114874609B CN 202210214570 A CN202210214570 A CN 202210214570A CN 114874609 B CN114874609 B CN 114874609B
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damping
parts
sheet material
piezoelectric ceramic
piezoelectric
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CN114874609A (en
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陈玉洁
陈文正
刘河洲
李华
余启立
范群福
郑栖潭
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Maanshan Economic And Technological Development Zone Construction Investment Co ltd
Shanghai Jiaotong University
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Maanshan Economic And Technological Development Zone Construction Investment Co ltd
Shanghai Jiaotong University
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    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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    • C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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    • E—FIXED CONSTRUCTIONS
    • E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
    • E01B—PERMANENT WAY; PERMANENT-WAY TOOLS; MACHINES FOR MAKING RAILWAYS OF ALL KINDS
    • E01B9/00—Fastening rails on sleepers, or the like
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Abstract

The invention relates to a high-damping intelligent vibration attenuation sheet material and a preparation method thereof, wherein the high-damping intelligent vibration attenuation sheet material comprises the following components in parts by mass: 30-90 parts of polytetramethylene glycol (PTMEG), 7.5-30 parts of polyol, 0.5-2.5 parts of isocyanate, 0-60 parts of Butyl Methacrylate (BMA), 0-60 parts of Methyl Methacrylate (MMA), 0-1 part of initiator, 20-40 parts of foam stabilizer, 0.05-0.5 part of MAX phase ceramic and 10-20 parts of piezoelectric ceramic. The preparation method comprises the following steps: self-assembling the piezoelectric ceramics and Mxens; mixing polytetramethylene glycol, polyalcohol, isocyanate, BMA, MMA and an initiator to prepare a polyurethane IPN matrix; and then the polyurethane IPN matrix, the piezoelectric ceramic/Mxenes self-assembled mixture and the foam homogenizing agent are subjected to prepolymerization, blending foaming, mould pressing and polarization to obtain the polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material. Compared with the prior art, the polyurethane IPN/piezoelectric ceramic/Mxenes high-damping intelligent vibration-damping sheet material has the characteristic of high damping, and expands the application of adding vibration-damping pads in the environment with vibration-damping requirements of the assembled ballastless track.

Description

High-damping intelligent vibration-damping sheet material and preparation method thereof
Technical Field
The invention belongs to the field of polymer composite materials, and particularly relates to a material preparation method of an assembled ballastless track high-damping intelligent vibration-damping pad accessory.
Background
In railways and track traffic, the ballasted track and the ballastless track can be judged according to the existence of a particle-free gravel track bed on a track base. The ballastless track adopts concrete and asphalt as the foundation of a ballast bed to transfer dynamic and static loads of a train during driving. The ballastless track has the advantages which the ballastless track does not have, wherein the ballastless track has the most remarkable advantage of good long-term stability so as to facilitate long-term service of the train under high-speed running. However, in general terms, the construction and maintenance of ballastless tracks has not been automated, and therefore additional costs are required for production and maintenance, and defects left during construction leave behind a risk for subsequent service life, thus requiring expensive costs to compensate.
With the development of the times, the mileage of the high-speed rail and the mileage of the urban rail are increased year by year, and accordingly, the maintenance requirements of the ballastless track and the requirements of paving new tracks are also greatly improved. However, according to recent literature reports, a prefabricated plate-type ballastless track system suitable for urban rail transit is introduced for adapting to more convenient urban rail transit construction. The system has the advantages of higher prefabrication precision, better quality, mechanized construction, high efficiency of on-site track laying, short construction period and the like. And the process is different from the process of cast-in-situ track bed, and the assembly and upgrading of the vibration reduction workpiece can be rapidly realized according to vibration reduction requirements when the track is prefabricated, so that the flexibility of the application of vibration reduction materials in the track traffic application is improved. In the novel assembly type ballastless track structure, a vibration reduction pad is designed between a self-compaction concrete pad layer and a base, the thickness of the vibration reduction layer is 30mm, polyurethane foam is generally used as a material, and a rubber material with a conical protrusion structure is used.
Under the background of the development of rail traffic engineering and science and the increasing demands for quality of life of people, the demands for reducing noise generated by high-speed operation of rail vehicles are also increasing gradually. On the one hand, in long-distance railway traffic, the use of ballastless tracks ensures that the running speed of a train is faster, and meanwhile, noise caused by the ballastless tracks causes a certain degree of interference to the ecological environment beside the rail and the living of rural residents; on the other hand, in short-distance urban rail transit, due to the fact that the track laying environment is complex, the urban environment is more sensitive to noise indexes, and the requirements of the construction of the urban rail transit on vibration reduction and noise reduction are higher. Meanwhile, the fatigue failure of the ballastless track is caused by continuous stress caused by most of driving trains, and cyclic stress caused by mechanical vibration in the running process of the trains, so that the fatigue crack is accelerated, the assembly components are loosened due to strong vibration, the cost of railway maintenance is increased, and the service life of the track is reduced.
Therefore, providing a high-damping intelligent vibration attenuation material for corresponding vibration attenuation pad accessories under the novel assembly type ballastless track technology is one of technical problems to be solved urgently by those skilled in the corresponding field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-damping intelligent vibration-damping sheet material and a preparation method thereof, and through self-assembly of Mxenes on piezoelectric ceramics, the surface electron transmission and the specific surface area of the piezoelectric ceramics after loading are improved, the bonding interface of particles and a high polymer matrix is improved, particle aggregation is prevented, the distribution of piezoelectric phases in the matrix is optimized, and therefore the overall damping performance is improved.
The aim of the invention can be achieved by the following technical scheme: a high-damping intelligent vibration attenuation sheet material comprises the following components in percentage by mass:
30-90 parts of polytetramethylene glycol (PTMEG), 7.5-30 parts of polyol, 0.5-2.5 parts of isocyanate, 0-60 parts of Butyl Methacrylate (BMA), 0-60 parts of Methyl Methacrylate (MMA), 0.2-1 part of initiator, 20-40 parts of foam stabilizer, 0.05-0.5 part of MAX phase ceramic and 10-20 parts of piezoelectric ceramic.
Further preferably, the high damping intelligent vibration attenuation sheet material comprises the following components in percentage by mass: 50-80 parts of polytetramethylene glycol (PTMEG), 15-25 parts of polyol, 1-2 parts of isocyanate, 20-40 parts of Butyl Methacrylate (BMA), 20-40 parts of Methyl Methacrylate (MMA), 0.2-0.6 part of initiator, 30-35 parts of foam stabilizer, 0.1-0.2 part of MAX phase ceramic and 15-18 parts of piezoelectric ceramic.
Further, the piezoelectric ceramic is lead titanate ceramic (PZT), and the grain size is 300nm-1000nm;
further, the initiator is azo initiator.
Further, the MAX phase ceramic is Ti 2 AlC ceramic particles.
The invention also provides a preparation method of the high-damping intelligent vibration-damping sheet material, wherein the high-damping intelligent vibration-damping sheet material takes Mxenes as a conductive phase, ceramic particles as a piezoelectric phase, polyurethane interpenetrating crosslinked network foam as a polyurethane IPN matrix, and the high-damping intelligent vibration-damping sheet material of polyurethane IPN/piezoelectric ceramic/Mxenes is obtained by self-assembling the Mxenes on the piezoelectric ceramic and then compounding the piezoelectric ceramic/the matrix.
Further, the Mxenes self-assemble on the piezoelectric ceramic as follows:
(1) Preparation of Mxenes2D sheets: adding MAX phase ceramic into NH 4 F and H 2 SO 4 Stirring for 20-30 h, then cleaning with deionized water, centrifuging, and pouring out supernatant to obtain a cleaned mixed solution with pH of 5-7;
(2) Stripping mxens 2D sheet: performing ultrasonic treatment on the mixed solution obtained in the step (1) for 1-3 h, performing centrifugal treatment for 10-30 min after the ultrasonic treatment is finished, taking the turbid solution on the upper layer as a stripped Mxene 2D lamellar aqueous solution, and sealing and preserving;
(3) Mxenes self-assembly: adding deionized water into piezoelectric ceramic particles, performing ultrasonic dispersion for 30-6 min, adding the stripped Mxene 2D lamellar aqueous solution in the step (2), stirring the mixed solution for 2-10 h to complete self-assembly, and sealing and preserving to obtain the piezoelectric ceramic/Mxene assembled suspension.
Further, NH in step (1) 4 F and H 2 SO 4 The molar ratio of (2) is 1-3:10-24; centrifuging at 8000-10000rad/min;
the speed of centrifugation in step (2) is 2000-4000rad/min;
the mass ratio of the piezoelectric ceramic to deionized water to the Mxenes2D lamellar aqueous solution in the step (3) is as follows: 10-20:20-50:10-20.
Further, the preparation method of the polyurethane IPN matrix comprises the following steps:
a) Primary blending: weighing polytetramethylene glycol, polyol and isocyanate according to the proportion, and blending for 20-30 min;
b) Secondary blending: weighing butyl methacrylate and methyl methacrylate according to the proportion, and blending with the blending liquid in the step a) for 20-30 min;
c) Three times blending of IPN: adding an initiator into the blending liquid obtained in the step b) to blend for 10-20 min, and sealing and preserving to obtain the polyurethane IPN matrix solution.
Further, the high-damping intelligent vibration attenuation sheet material is prepared by the following steps:
i) Prepolymerization: preserving the temperature of the polyurethane IPN matrix solution at 70-80 ℃ for 4-8 hours to finish the prepolymerization;
ii) four-time compounding blending: mixing the piezoelectric ceramic/Mxenes assembled suspension with the pre-polymerized blend in the step i) to obtain a mixture with the weight ratio of 1:100-20:100, adding 20-40 parts by mass of a foam homogenizing agent CGY-3, stirring for foaming, pouring into a mould and closing the mould;
iii) Final polymerization: preserving heat for 10-14 h at 120-150 ℃ after die assembly;
iv) cooling: opening a die, and cooling the vibration damping sheet material for 1-2 h at room temperature;
v) polarization: and (3) carrying out polarization treatment on the piezoelectric damping composite material obtained in the step (iv) to finally obtain the polyurethane IPN/piezoelectric ceramic/Mxene high-damping intelligent vibration attenuation sheet material.
The polarization treatment is as follows: copper electrodes are stuck on two sides of the surface of the piezoelectric damping composite material, and the piezoelectric damping composite material is polarized for 30min in the environment of 60 ℃ silicone oil at the speed of 3kv/mm-5 kv/mm.
Compared with the prior art, the invention has the following beneficial effects:
in the macromolecule-based vibration reduction composite material, the piezoelectric damping material has the unique advantages of an intelligent vibration reduction material, firstly, the piezoelectric damping material is composed of a macromolecule matrix, piezoelectric ceramics and conductive phases, the piezoelectric ceramics particles generate charges on the surface under vibration load, the conductive phases in the composite material transmit electrons to form a conductive path, and due to the Joule heat effect of the resistor under the conductive path, the energy conversion of converting mechanical vibration energy into electric energy and then into heat energy is realized, and finally, the effect of improving the damping performance of the piezoelectric damping composite material is realized. Meanwhile, in the application of the ballastless track vibration-damping pad, the piezoelectric composite material can be used as a sensor to detect incoming vibration, the defect and fatigue degree of adjacent components can be diagnosed according to the change of the vibration, the intellectualization of the vibration-damping material is truly realized, and the maintenance and detection cost of the ballastless track is reduced to a certain extent.
The Mxenes as 2D material has excellent electromagnetic property, high specific surface area and adsorptivity, and can be used as filler to prepare intelligent high molecular composite material with high performance, and the conductivity, thermal conductivity, mechanical property and flame retardance of high molecular are improved. Meanwhile, a large number of active ends exist in the process of etching the MAX by HF, so that the interface between the Mxenes and the polymer matrix is well combined, and the layer space is adjusted, thereby providing favorable conditions for preparing the polymer/Mxenes composite material.
According to the intelligent vibration-damping piezoelectric damping composite material, the Mxenes is used as a conductive phase, the PZT ceramic particles are used as a piezoelectric phase, the polyurethane interpenetrating crosslinked network foam is used as a matrix, and the self-assembly of the Mxenes on the piezoelectric ceramic is used for improving the surface electron transmission and the specific surface area of the piezoelectric ceramic after loading, improving the bonding interface of the particles and a high polymer matrix, preventing particle aggregation, optimizing the distribution of the piezoelectric phase in the matrix, so that the overall damping performance is improved, and the application of the assembled ballastless track in adding vibration-damping pads in an environment with vibration-damping requirements is expanded.
Drawings
FIG. 1 is a flow chart of the self-assembly of Mxenes on piezoelectric ceramics according to the present invention;
FIG. 2 is a flow chart of the process for manufacturing the polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration damping sheet material;
FIG. 3 is a graph of polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material loss factor;
FIG. 4 is a graph of the storage modulus of polyurethane IPN/piezoelectric ceramic/Mxenes high damping smart damping sheet material;
FIG. 5 is a graph of the loss modulus of a polyurethane IPN/piezoelectric ceramic/Mxenes high damping smart damping sheet material.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
It should be noted that, without conflict, the embodiments of the present invention related to the preparation of the IPN base and the features in the embodiments may be combined with each other. The invention is further described below with reference to examples, the loss factors of the obtained polyurethane IPN/piezoelectric ceramic/Mxens high-damping intelligent vibration-damping sheet material of the embodiment are shown in FIG. 3, the storage modulus of the obtained polyurethane IPN/piezoelectric ceramic/Mxens high-damping intelligent vibration-damping sheet material of the embodiment is shown in FIG. 4, the loss modulus of the obtained polyurethane IPN/piezoelectric ceramic/Mxens high-damping intelligent vibration-damping sheet material of the embodiment is shown in FIG. 5, and the loss coefficients of the obtained polyurethane IPN/piezoelectric ceramic/Mxens high-damping intelligent vibration-damping sheet material of the embodiment at characteristic temperatures are compared with each other in Table 1. The embodiment is implemented on the premise of the technical scheme of the invention, and a detailed implementation method and a specific operation process are provided, but the protection scope of the invention is not limited to the following implementation cases.
The invention provides a preparation method of a polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material, which comprises the following steps:
1. piezoelectric ceramics/Mxenes self-assemble as shown in fig. 1:
(1) Preparation of Mxenes2D sheets: MAX phase (Ti) is added according to the proportion 2 AlC) ceramic, requiring addition of 0.5mol to 1.5mol NH 4 F and 5mol-12mol H 2 SO 4 Wherein HF (hydrofluoric acid) and Ti are in situ 2 Mole ratio of AlC 9:1, stirring 2Washing with deionized water for 0-30 hr, centrifuging at 8000-10000rad/min, and removing supernatant to obtain mixed solution with pH of 5-7;
(2) Stripping mxens 2D sheet: treating the mixed solution obtained in the step (1) for 1-3 h by ultrasonic treatment, centrifuging for 10-30 min by 2000-4000rad/min after the ultrasonic treatment, taking the upper turbid solution as stripped Mxenes2D lamellar aqueous solution, and sealing and preserving;
(3) Mxenes self-assembly: adding 10-20 parts by mass of piezoelectric ceramic (PZT) particles according to a proportion, adding 20-50 parts by mass of deionized water, performing ultrasonic dispersion for 30-6 min, simultaneously adding 10-20 parts by mass of the stripped Mxenes2D lamellar aqueous solution in the step (2), and finally stirring the mixed solution for 2-10 h to complete self-assembly, and sealing and preserving.
2. Preparation of polyurethane IPN matrix as shown in FIG. 2
(4) Primary blending: weighing polytetramethylene glycol, polyol and isocyanate according to the proportion, and blending for 20-30 min;
(5) Secondary blending: weighing butyl methacrylate and methyl methacrylate according to the proportion, and blending with the blending liquid in the step (4) for 20-30 min;
(6) Three times blending of IPN: adding the initiator into the liquid blended in the step (5), blending for 10-20 min, and sealing and preserving.
3. Preparation of polyurethane IPN/piezoelectric ceramic/Mxene high damping intelligent vibration attenuation sheet material
(7) Prepolymerization: preserving the temperature of the blending solution obtained in the step (6) at 70-80 ℃ for 4-8 hours to finish the prepolymerization;
(8) Four-time compound blending: mixing the self-assembled suspension in the step (3) with the pre-polymerized blend in the step (7) to obtain a mixture with the weight ratio of 1:100-20:100, adding 20-40 parts by mass of a foam homogenizing agent CGY-3, stirring for foaming, pouring into a mould and closing the mould;
(9) Final polymerization: after die assembly, preserving heat for 10-14 h at 120-150 ℃;
(10) And (3) cooling: cooling the vibration damping sheet material for 1-2 h at room temperature after die opening is required;
(11) Polarization: and (3) sticking copper electrodes on two sides of the surface of the piezoelectric damping composite material obtained in the step (10), and polarizing the piezoelectric damping composite material for 30min at the temperature of 60 ℃ in the environment of 3-5 kv/mm. Finally, the polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material is obtained.
Specific examples in the following examples, the amounts of the respective components are measured in parts by weight unless otherwise specified.
Comparative example 1
1) Weighing 20g of PZT ceramic particles, adding 50g of deionized water, performing ultrasonic dispersion for 30min to obtain a suspension, and sealing for later use.
2) 41g of polytetramethylene glycol (PTMEG), 7.5g of glycerol, 0.5g of diphenylmethane-4, 4' -diisocyanate (MDI), PTMEG and glycerol monomers were weighed out; the diphenylmethane-4, 4' -diisocyanate (MDI) monomer is heated to 60 ℃ until the monomer is melted into colorless transparent liquid, and the three monomers are blended to obtain PU for standby.
3) The mass ratio of Methyl Methacrylate (MMA) monomer, (butyl methacrylate) BMA monomer to Polyurethane (PU) in step 2) was weighed to be PU: BMA: mma=1:2:1, where PU 25g,BMA 50g,MMA 25g. After blending of MMA and BMA monomers, 0.15g of Azobenzene (AIBN) is required as an initiator, and the mixture is heated in an oil bath at 60 ℃ until the monomer mixture is in an oily liquid with viscosity for later use.
4) Preserving the temperature of the blend in the step 3) at 70-80 ℃ for more than 4 hours to finish initial polymerization, and then adding the suspension in the step 1), wherein the mass ratio of the suspension to the initial polymer is 20:100, 35g of foam stabilizer CGY-3 is added, stirred and foamed, poured into a mold, and the mold is closed and placed into an oven.
5) Preserving the temperature for 14h at 120-140 ℃ to finish final polymerization, and cooling for 2h at room temperature after die opening.
6) And (3) attaching copper electrodes to two sides of the material obtained in the step (5), and polarizing the material for 30min in a silicone oil environment at 60 ℃ according to a polarization system of 4kv/mm to obtain a comparative example material 1.
Example 1
A preparation method of a high-damping intelligent vibration attenuation sheet material comprises the following steps:
1) Weigh 0.5g Ti 2 Adding 1mol NH4F and 9mol concentrated sulfuric acid into AlC ceramic particles, and stirring for 24 hours in a plastic beaker and in a ventilation environment; the mixture was then rinsed with deionized water to 1Centrifugation is carried out for 15min at 0000rad/min, and new deionized water is added after the supernatant is poured off. This was repeated six times.
2) Further, the cleaned mixed solution is subjected to ultrasonic treatment for 1 hour, then the Mxenes2D sheet layer is peeled off, and then centrifugation is carried out for 30 minutes at 3500rad/min, and supernatant fluid is removed to obtain an aqueous solution of the Mxenes2D sheet layer.
3) Weighing 20g of ceramic Particles (PZT), adding 50 parts of deionized water, performing ultrasonic dispersion for 30min to obtain a suspension, adding 10g of the suspension in the step 2) to obtain an Mxene 2D lamellar aqueous solution, stirring for 10h to realize self-assembly, obtaining a mixed suspension after completion, and sealing for later use.
4) 41g of polytetramethylene glycol (PTMEG), 7.5g of glycerol, 0.5g of diphenylmethane-4, 4' -diisocyanate (MDI), PTMEG and glycerol monomers were weighed out; the diphenylmethane-4, 4' -diisocyanate (MDI) monomer is heated to 60 ℃ until the monomer is melted into colorless transparent liquid, and the three monomers are blended to obtain PU for standby.
5) The mass ratio of Methyl Methacrylate (MMA) monomer, (butyl methacrylate) BMA monomer to Polyurethane (PU) in step 4) was weighed to be PU: BMA: mma=1:2:1, where PU 25g,BMA 50g,MMA 25g. After blending of MMA and BMA monomers, 0.15g of Azobenzene (AIBN) is required as an initiator, and the mixture is heated in an oil bath at 60 ℃ until the monomer mixture is in an oily liquid with viscosity for later use.
6) Preserving the temperature of the blend in the step 5) at 70-80 ℃ for more than 4 hours to finish initial polymerization, and then adding the suspension in the step 3), wherein the mass ratio of the suspension to the initial polymer is 20:100, 35g of foam stabilizer CGY-3 is added, stirred and foamed, poured into a mold, and the mold is closed and placed into an oven.
7) Preserving the temperature for 14h at 120-140 ℃ to finish final polymerization, and cooling for 2h at room temperature after die opening.
8) And (3) attaching copper electrodes to two sides of the material obtained in the step (5), and polarizing the material for 30min in a silicone oil environment at 60 ℃ according to a polarization system of 4kv/mm to obtain the example material 1.
Example 2
A preparation method of a high-damping intelligent vibration attenuation sheet material comprises the following steps:
1) 0.5g of Ti2AlC ceramic particles are weighed, 1mol NH4F and 9mol concentrated sulfuric acid are added, and the mixture is stirred for 24 hours in a plastic beaker and in a ventilation environment; the mixture was then rinsed with deionized water, centrifuged at 10000rad/min for 15min, and the supernatant was decanted and fresh deionized water was added. This was repeated six times.
2) Further, the cleaned mixed solution is subjected to ultrasonic treatment for 1 hour, then the Mxenes2D sheet layer is peeled off, and then centrifugation is carried out for 30 minutes at 3500rad/min, and supernatant fluid is removed to obtain an aqueous solution of the Mxenes2D sheet layer.
3) Weighing 20g of ceramic particles, adding 50g of deionized water, performing ultrasonic dispersion for 30min to obtain a suspension, adding 15g of the suspension in the step 2) to obtain an Mxene 2D lamellar aqueous solution, stirring for 10h to realize self-assembly, obtaining a mixed suspension after completion, and sealing for later use.
4) 41g of polytetramethylene glycol (PTMEG), 7.5g of glycerol, 0.5g of diphenylmethane-4, 4' -diisocyanate (MDI), PTMEG and glycerol monomers were weighed out; diphenylmethane-4, 4' -diisocyanate (MDI) monomer was heated to 60 ℃ until it was melted to a colorless transparent liquid. Three monomers are blended for standby.
5) The mass ratio of Methyl Methacrylate (MMA) monomer, (butyl methacrylate) BMA monomer to Polyurethane (PU) in step 4) was weighed to be PU: BMA: mma=1:2:1, where PU 25g,BMA 50g,MMA 25g. After blending of MMA and BMA monomers, 0.15g of Azobenzene (AIBN) is required as an initiator, and the mixture is heated in an oil bath at 60 ℃ until the monomer mixture is in an oily liquid with viscosity for later use.
6) Preserving the temperature of the blend in the step 5) at 70-80 ℃ for more than 4 hours to finish initial polymerization, and then adding the suspension in the step 3), wherein the mass ratio of the suspension to the initial polymer is 20:100, 35g of foam stabilizer CGY-3 is added, stirred and foamed, poured into a mold, and the mold is closed and placed into an oven.
7) Preserving the temperature for 14h at 120-140 ℃ to finish final polymerization, and cooling for 2h at room temperature after die opening.
8) And (3) attaching copper electrodes to two sides of the material obtained in the step (5), and polarizing the material for 30min in a silicone oil environment at 60 ℃ according to a polarization system of 4kv/mm to obtain the example material 2.
Example 3
1) 0.5g of Ti2AlC ceramic particles are weighed, 1mol NH4F and 9mol concentrated sulfuric acid are added, and the mixture is stirred for 24 hours in a plastic beaker and in a ventilation environment; the mixture was then rinsed with deionized water, centrifuged at 10000rad/min for 15min, and the supernatant was decanted and fresh deionized water was added. This was repeated six times.
2) And (3) carrying out ultrasonic treatment on the cleaned mixed solution for 1h, then stripping the Mxene 2D sheet, centrifuging at 3500rad/min for 30min, and removing the supernatant to obtain an aqueous solution of the Mxene 2D sheet.
3) Weighing 20g of ceramic particles, adding 50g of deionized water, performing ultrasonic dispersion for 30min to obtain a suspension, adding 20g of the suspension in the step 2) to obtain an Mxene 2D lamellar aqueous solution, stirring for 10h to realize self-assembly, obtaining a mixed suspension after completion, and sealing for later use.
4) 41g of polytetramethylene glycol (PTMEG), 7.5g of glycerol, 0.5g of diphenylmethane-4, 4' -diisocyanate (MDI), PTMEG and glycerol monomers were weighed out; diphenylmethane-4, 4' -diisocyanate (MDI) monomer was heated to 60 ℃ until it was melted to a colorless transparent liquid. Three monomers are blended for standby.
5) The mass ratio of Methyl Methacrylate (MMA) monomer, (butyl methacrylate) BMA monomer to Polyurethane (PU) in step 4) was weighed to be PU: BMA: mma=1:2:1, where PU 25g,BMA 50g,MMA 25g. After blending of MMA and BMA monomers, 0.15g of Azobenzene (AIBN) is required as an initiator, and the mixture is heated in an oil bath at 60 ℃ until the monomer mixture is in an oily liquid with viscosity for later use.
6) Preserving the temperature of the blend in the step 5) at 70-80 ℃ for more than 4 hours to finish initial polymerization, and then adding the suspension in the step 3), wherein the mass ratio of the suspension to the initial polymer is 20:100, 35g of foam stabilizer CGY-3 is added, stirred and foamed, poured into a mold, and the mold is closed and placed into an oven.
7) Preserving the temperature for 14h at 120-140 ℃ to finish final polymerization, and cooling for 2h at room temperature after die opening.
8) Attaching copper electrodes to two sides of the material obtained in the step 5), and polarizing for 30min at 60 ℃ in a silicone oil environment according to a polarization system of 4kv/mm to obtain a material 3 of the example
The materials obtained in the comparative examples and examples were subjected to performance tests as follows: the resulting polyurethane IPN/piezoelectric ceramic/mxens high damping intelligent vibration attenuation sheet was cut into a sheet having dimensions (length, width, thickness) of 10mm×2mm×1mm, and performance test was performed using a dynamic thermo-mechanical analyzer (Q800, usa), and the test results are shown in table 1 below:
TABLE 1 loss factor at specific temperature for polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet materials
Sample name 0℃ 10℃ 20℃ 30℃ 40℃ 50℃
Comparative example 1 0.12226 0.13324 0.14680 0.15364 0.15503 0.15181
Example 1 1.16602 0.82211 0.54659 0.34639 0.22284 0.13657
Example 2 0.83934 0.88376 0.77607 0.60816 0.44794 0.31596
Example 3 0.81394 0.89308 0.81844 0.64546 0.46464 0.32489
FIG. 3 is a graph showing the loss factor of polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration damping sheet material, and it can be seen from the graph that the Mxenes conductive phase is not added in comparative example 1, the peak loss factor of the graphs of examples 1-3 moves to high temperature, the temperature zone of loss factor tan delta >0.8 is increased, the glass transition temperature is increased, the use condition of room temperature or higher is more met, and the temperature zone of tan delta >0.6 in the graph is widened.
FIG. 4 shows the storage modulus of the polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration damping sheet material, and it can be seen from the figure that the storage modulus of the graph of the example 1-3 is obviously improved in the low temperature region without adding the Mxenes conductive phase, and the material shows higher storage modulus after adding the Mxenes conductive phase in the normal temperature region.
FIG. 5 shows the loss modulus of the polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration damping sheet material, and from the graph, it can be seen that the loss modulus of the example 1-3 graph is obviously improved in the low temperature region without adding the Mxenes conductive phase, and the material shows higher loss modulus after adding the Mxenes conductive phase in the normal temperature region.
Example 4
A preparation method of a polyurethane/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material comprises the following steps:
1. piezoelectric ceramics/Mxenes self-assemble as shown in fig. 1:
(1) Preparation of Mxenes2D sheets: MAX phase (Ti) is added according to the proportion 2 AlC) ceramic 0.05g, requiring addition of 0.5molmol NH 4 F and 5mol H 2 SO 4 Wherein HF (hydrofluoric acid) and Ti are in situ 2 Mole ratio of AlC 9:1, stirring for 20h, then cleaning by using deionized water, centrifuging at 8000rad/min, and pouring out supernatant, wherein the pH of the mixed solution is required to be 5;
(2) Stripping mxens 2D sheet: treating the mixed solution obtained in the step (1) for 1h by ultrasonic treatment, centrifuging for 10min by 2000rad/min after the ultrasonic treatment is finished, taking the turbid solution on the upper layer as stripped Mxene 2D lamellar aqueous solution, and sealing and preserving;
(3) Mxenes self-assembly: adding 10g of piezoelectric ceramic (PZT) particles according to a proportion, adding 20g of deionized water, performing ultrasonic dispersion for 30-6 min, simultaneously adding 10g of the stripped Mxene 2D lamellar aqueous solution in the step (2), and finally stirring the mixed solution for 2h to complete self-assembly, and sealing and preserving.
2. Preparation of polyurethane matrix as shown in FIG. 2
(4) Primary blending: weighing 30g of polytetramethylene glycol, 10g of polyol and 0.5g of isocyanate according to the proportion, and blending for 20min;
(7) Secondary blending of polyurethane: continuously blending the liquid blended in the step (4) for 10min, and sealing and preserving
3. Preparation of polyurethane/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material
(6) Prepolymerization: preserving the heat of the blending solution obtained in the step (6) for 4 hours at 70 ℃ to finish the prepolymerization;
(7) Three times of compound blending: mixing the self-assembled suspension in the step (3) with the pre-polymerized blend in the step (7) to obtain a mixture with the weight ratio of 1:20, adding 20g of foam homogenizing agent CGY-3, stirring for foaming, and pouring into a mould for mould closing;
(8) Final polymerization: after die assembly, preserving heat for 14h at 120 ℃;
(9) And (3) cooling: cooling the vibration damping sheet material for 1h at room temperature after die opening is required;
(10) Polarization: and (3) sticking copper electrodes on two sides of the surface of the piezoelectric damping composite material obtained in the step (10), and polarizing for 30min at the temperature of 60 ℃ in a silicone oil environment of 3 kv/mm. Finally, the polyurethane/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material is obtained.
Example 5
A preparation method of a polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material comprises the following steps:
1. piezoelectric ceramics/Mxenes self-assemble as shown in fig. 1:
(1) Preparation of Mxenes2D sheets: MAX phase (Ti) is added according to the proportion 2 AlC) ceramic 0.5g, 1.5mol NH is required to be added 4 F and 12mol H 2 SO 4 Wherein HF (hydrofluoric acid) and Ti are in situ 2 Mole ratio of AlC 9:1, stirring for 30h, then cleaning by using deionized water, centrifuging at 10000rad/min, and pouring out supernatant, wherein the pH of the mixed solution is required to be 7;
(2) Stripping mxens 2D sheet: subjecting the mixed solution obtained in the step (1) to ultrasonic treatment for 3 hours, centrifuging at 4000rad/min for 30min after the ultrasonic treatment is finished, taking the turbid solution at the upper layer as stripped Mxene 2D lamellar aqueous solution, and sealing and preserving;
(3) Mxenes self-assembly: and (3) adding 20g of piezoelectric ceramic (PZT) particles according to a proportion, adding 50g of deionized water, performing ultrasonic dispersion for 6min, simultaneously adding 20g of the stripped Mxenes2D lamellar aqueous solution in the step (2), and finally stirring the mixed solution for 10h to complete self-assembly, and sealing and preserving.
2. Preparation of polyurethane IPN matrix as shown in FIG. 2
(4) Primary blending: weighing 90g of polytetramethylene glycol, 30g of polyol and 2.5g of isocyanate according to the proportion, and blending for 30min;
(5) Secondary blending: weighing 60g of butyl methacrylate and 60g of methyl methacrylate according to the proportion, and blending with the blending liquid in the step (4) for 30min;
(6) Three times blending of IPN: and (3) adding 1g of Azobenzene (AIBN) serving as an initiator into the liquid blended in the step (5), blending for 20min, and sealing and preserving.
3. Preparation of polyurethane IPN/piezoelectric ceramic/Mxene high damping intelligent vibration attenuation sheet material
(7) Prepolymerization: preserving the heat of the blending solution obtained in the step (6) for 8 hours at 80 ℃ to finish the prepolymerization;
(8) Four-time compound blending: mixing the self-assembled suspension in the step (3) and the pre-polymerized blend in the step (7) by 10:100, adding 40g of foam homogenizing agent CGY-3, stirring for foaming, pouring into a mould and closing;
(9) Final polymerization: after die assembly, preserving heat for 10 hours at 150 ℃;
(10) And (3) cooling: cooling the vibration damping sheet material for 2 hours at room temperature after die opening is required;
(11) Polarization: and (3) sticking copper electrodes on two sides of the surface of the piezoelectric damping composite material obtained in the step (10), and polarizing for 30min at the temperature of 60 ℃ in a silicone oil environment of 5 kv/mm. Finally, the polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet material is obtained.
The materials obtained in examples 4 to 5 were tested using the following test method of example 1: the resulting polyurethane IPN/piezoceramic/mxens high damping intelligent vibration attenuation sheet was cut into 10mm x 2mm x 1mm sized (length, width, thickness) sheets and performance tested using a dynamic thermo-mechanical analyzer (Q800, usa) with the results shown in table 2 below:
TABLE 2 loss factor at specific temperature for polyurethane IPN/piezoelectric ceramic/Mxenes high damping intelligent vibration attenuation sheet materials
0℃ 10℃ 20℃ 30℃
Example 4 0.2247 0.1824 0.0232 0.0157
Example 5 0.2546 0.2354 0.2232 0.2323
As can be seen from table 2 above, when BMA and MMA are not added, the polyurethane/piezoelectric ceramic/Mxenes high damping smart damping patch material formed is much lower than example 3 at room temperature; from the data in example 5 in the table, it can be seen that the loss is lower at room temperature range when BMA and MMA are added to the end values.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (7)

1. The high-damping intelligent vibration attenuation sheet material is characterized by comprising the following components in parts by mass:
30-90 parts of polytetramethylene glycol, 7.5-30 parts of polyalcohol, 0.5-2.5 parts of isocyanate, 20-60 parts of Butyl Methacrylate (BMA), 20-60 parts of Methyl Methacrylate (MMA), 0.2-1 part of initiator, 20-40 parts of foam stabilizer, 0.05-0.5 part of MAX phase ceramic and 10-20 parts of piezoelectric ceramic; the initiator is azo initiator;
the high-damping intelligent vibration attenuation sheet material takes Mxenes as a conductive phase, piezoelectric ceramic as a piezoelectric phase, polyurethane interpenetrating crosslinked network foam as a polyurethane IPN matrix, and is obtained by self-assembling the Mxenes on the piezoelectric ceramic and then compositing the piezoelectric ceramic with the matrix;
the Mxenes self-assemble on piezoelectric ceramics as follows:
(1) Preparation of Mxenes2D sheets: adding MAX phase ceramic into NH 4 F and H 2 SO 4 Stirring for 20-30 h, then cleaning with deionized water, centrifuging, and pouring out supernatant to obtain a cleaned mixed solution with pH of 5-7;
(2) Stripping mxens 2D sheet: performing ultrasonic treatment on the mixed solution obtained in the step (1) for 1-3 h, performing centrifugal treatment for 10-30 min after the ultrasonic treatment is finished, taking the turbid solution on the upper layer as a stripped Mxene 2D lamellar aqueous solution, and sealing and preserving;
(3) Mxenes self-assembly: adding deionized water into piezoelectric ceramic particles, performing ultrasonic dispersion for 30-6 min, adding the stripped Mxene 2D lamellar aqueous solution in the step (2), stirring the mixed solution for 2-10 h to complete self-assembly, and sealing and preserving to obtain piezoelectric ceramic/Mxene assembled suspension;
the preparation method of the polyurethane IPN matrix comprises the following steps:
a) Primary blending: weighing polytetramethylene glycol, polyol and isocyanate according to the proportion, and blending for 20-30 min;
b) Secondary blending: weighing butyl methacrylate and methyl methacrylate according to the proportion, and blending with the blending liquid in the step a) for 20-30 min;
c) Three times blending of IPN: adding an initiator into the blending liquid obtained in the step b) to blend for 10-20 min, and sealing and preserving to obtain the polyurethane IPN matrix solution.
2. The high-damping intelligent vibration attenuation sheet material according to claim 1, wherein the high-damping intelligent vibration attenuation sheet material comprises the following components in parts by mass: 50-80 parts of polytetramethylene glycol, 15-25 parts of polyalcohol, 1-2 parts of isocyanate, 20-40 parts of Butyl Methacrylate (BMA), 20-40 parts of Methyl Methacrylate (MMA), 0.2-0.6 part of initiator, 30-35 parts of foam stabilizer, 0.1-0.2 part of MAX phase ceramic and 15-18 parts of piezoelectric ceramic.
3. The high-damping intelligent vibration attenuation sheet material according to claim 1, wherein the piezoelectric ceramic is lead zirconate titanate ceramic (PZT) with a grain size of 300nm-1000nm.
4. The high-damping intelligent vibration attenuation sheet material according to claim 1, wherein said MAX phase ceramic is Ti 2 AlC ceramic particles.
5. The high damping intelligent vibration attenuation sheet material according to claim 1, wherein in step (1), NH 4 F and H 2 SO 4 The molar ratio of (2) is 1-3:10-24; centrifuging at 8000-10000rad/min;
the speed of centrifugation in step (2) is 2000-4000rad/min;
the mass ratio of the piezoelectric ceramic to deionized water to the Mxenes2D lamellar aqueous solution in the step (3) is as follows: 10-20:20-50:10-20.
6. The high-damping intelligent vibration attenuation sheet material according to claim 1, wherein the high-damping intelligent vibration attenuation sheet material is prepared by the following method:
i) Prepolymerization: preserving the temperature of the polyurethane IPN matrix solution at 70-80 ℃ for 4-8 hours to finish the prepolymerization;
ii) four-time compounding blending: combining the piezoelectric ceramic/Mxenes assembled suspension with the pre-polymerized blend of step i) to 20:100, adding 20-40 parts by mass of foam homogenizing agent, stirring and foaming, and pouring into a mould for mould closing;
iii) Final polymerization: preserving heat for 10-14 h at 120-150 ℃ after die assembly;
iv) cooling: opening a die, and cooling the vibration damping sheet material for 1-2 h at room temperature to obtain a piezoelectric damping composite material;
v) polarization: and (3) carrying out polarization treatment on the piezoelectric damping composite material obtained in the step (iv) to finally obtain the polyurethane IPN/piezoelectric ceramic/Mxene high-damping intelligent vibration attenuation sheet material.
7. The high damping intelligent vibration attenuation sheet material according to claim 6, wherein said polarization treatment is: copper electrodes are stuck on two sides of the surface of the piezoelectric damping composite material, and the piezoelectric damping composite material is polarized for 30min in the environment of 60 ℃ silicone oil at the speed of 3kv/mm-5 kv/mm.
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