CN103881253A - Piezoelectric damping material using polypyrrole as conductive channel and preparation method thereof - Google Patents
Piezoelectric damping material using polypyrrole as conductive channel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a piezoelectric damping material using polypyrrole as a conductive channel, which is prepared from the following components in parts by weight: 100 parts of rubber, 1-5 parts of accelerator, 1-5 parts of sulfur, 1-3 parts of anti-aging agent, 50-200 parts of mica powder, 10-100 parts of epoxy resin and 100-1000 parts of polypyrrole/piezoelectric ceramic powder composite material. The polypyrrole/piezoelectric ceramic powder composite material comprises the following components in parts by weight: 100 parts of piezoelectric ceramic powder, 30-60 parts of pyrrole monomer and 15-30 parts of initiator. The maximum loss factor (tan delta max) of the piezoelectric damping material is greater than or equal to 0.7, the effective damping temperature range (Delta T0.7) is greater than or equal to 40 DEG C, the loss factor (tan alpha) at 30 DEG C under the frequency of 1-1000Hz is greater than or equal to 0.5, and the temperature range is 20-100 DEG C when the frequency range is 1-1000Hz and the loss factor (tank alpha) is greater than or equal to 0.3.
Description
Technical field
The invention belongs to functional composite material field, especially relate to a kind of poly-arsenic and press against piezo-electric damping material and the preparation method into conductive channel.
Background technology
Known, piezo-electric damping material is in macromolecular material, to insert piezoelectric filler and conductive filler material, in the time that material is subject to vibrating, piezoelectric filler can change vibrational energy into electric energy, changing electric energy into thermal dissipation by conductive filler material again goes out, reach the object of vibration damping, its principle is to utilize the viscous-elastic behaviour of macromolecular material and the piezoelectric effect of piezoelectric filler, realizes mechanical energy-electric energy-Re conversion of energy.
Most of patents (publication number CN 101191000A, CN101486811A, CN101649073A, CN101328302A, CN101392090A) piezo-electric damping material of invention adopts graphitized carbon black, graphite, carbon fiber, carbon nanotube as conductive filler material, mode by mechanical blending is blended into conductive filler material in piezo-electric damping material, forms the conductive channel of a series of microcosmic between conductive filler material and piezoelectric ceramic powder by the mode of mechanical blending, realizes electric energy to hot conversion of energy.
Adopt graphitized carbon black, graphite, carbon fiber, carbon nanotube as conductive filler material, although can realize piezo-electric damping material conversion process of energy, need in polymeric matrix, add a large amount of conductive filler materials.In the time containing a large amount of conductive filler materials in piezo-electric damping material, because the specific conductivity of conductive filler material is certain, piezo-electric damping material will have very strong frequency dependence, is not suitable for making the damping material of wideband.In addition, between conductive filler material and piezoelectric ceramic powder, be to combine by the mode of mechanical blending, this mode can cause conductive filler material and piezoelectric ceramic powder separately between a large amount of gatherings, can not give full play to the energy transformation effect of each piezoelectric ceramic powder, can efficiency of conversion a little less than, damping capacity is poor.
Summary of the invention
In order to overcome the deficiency in background technology, the invention discloses a kind of poly-press against/piezoelectric ceramic powder composite material of arsenic and preparation method, and piezo-electric damping material and preparation method take the press against/piezoelectric ceramic powder composite material that gathers arsenic as conductive channel.
In order to realize described goal of the invention, the present invention adopts following technical scheme:
A kind of poly-arsenic is pressed against the piezo-electric damping material into conductive channel, described piezo-electric damping material component be by weight: 100 parts of rubber, 1～5 part of promotor, 1～5 part, sulphur, 1～3 part, anti-aging agent, 50～200 parts of mica powders, 10～100 parts of epoxy resin, 100～1000 parts of press against/piezoelectric ceramic powder composite materials of poly-arsenic; Wherein said press against/piezo-electric ceramic composite material of poly-arsenic component be by weight: 100 parts of piezoelectric ceramic powders, arsenic is pressed against 30～60 parts of monomers, 15～30 parts of initiators; Described piezoelectric ceramic powder is the one in magnesium niobium lead zirconate titanate type piezoelectric ceramics, Pb-based lanthanumdoped zirconate titanates type piezoelectric ceramics or modification magnesium niobium lead zirconate titanate type piezoelectric ceramics.
Rubber of the present invention is the one in paracril, natural rubber, chlorosulfonated polyethylene, urethanes.
Promotor of the present invention is one or both in dibenzothiazyl disulfide DM, vulkacit D D and tetramethyl-dithio thiuram TMTD.
Anti-aging agent of the present invention is the one in antioxidant 4010NA, antioxidant A W, antioxidant D.
Mica powder of the present invention is one or both in 80 orders, 200 orders and 325 orders.
Epoxy resin of the present invention is one or both in E-51, E-44.
The particle diameter of piezoelectric ceramic powder of the present invention is 1-10um.
A preparation method for press against/piezoelectric ceramic powder composite material of poly-arsenic, uses chemical oxidation situ aggregation method, comprises the following steps:
(1) obtain solution: first add piezoelectric ceramic powder in there-necked flask, then there-necked flask is fixed on the iron stand with whipping appts, flask approximately 3/4ths parts are immersed in the water bath with thermostatic control of 70 ℃～80 ℃, turn on agitator, in there-necked flask, add distilled water again, the material being bonded in flask walls is poured to there-necked flask bottom, itself and distilled water are mixed.After 70 ℃～80 ℃ constant temperature 10～20min of water-bath, under whipped state, first arsenic is pressed against gradually and joined in there-necked flask, then hydrochloric acid is joined in there-necked flask gradually, stir and obtain black mixing solutions;
(2) isothermal reaction: under strong stirring, constant temperature water bath reaction is carried out 24 ~ 28 hours;
(3) aftertreatment: after having reacted, close water-bath, after question response thing is cooling, filter with vacuum filtration device, then use absolute ethanol washing, generally wash 3 ~ 4 times, obtain black powder, now powder is hygrometric state and is bonded together.The black powder obtaining is encased in culture dish, under state of nature, ethanol is volatilized gradually, generally need 24 ~ 48 hours according to envrionment temperature, then grind black powder with mortar it is scatter, then material is put in the baking oven of 100 ℃～110 ℃ dry 2～3 hours.
Poly-arsenic is pressed against the piezo-electric damping material into conductive channel, comprises the following steps:
(1) preparation of blank: by formula, after rubber is plasticated in mill, add poly-press against/piezoelectric ceramic powder composite material of arsenic, epoxy resin, mica powder, anti-aging agent, promotor, sulphur, mixing even;
(2) sulfuration: be 10～12MPa by blank pressure in metal die, temperature is 150～160 ℃, and curing time is that under 20～40min condition, sulfidization molding becomes sizing material;
(3) polarization: conductive silver glue is stirred, with the even sizing material two sides of brushing at sulfidization molding of hairbrush, be dry 2～3h in the loft drier of 100～120 ℃ in temperature, after cooling in room temperature environment, putting into high voltage direct current oil bath device polarizes again, strength of electric field is 1～3kv/mm, and polarization 20～30min, can obtain piezo-electric damping material of the present invention.
Owing to having adopted technique scheme, the present invention has following beneficial effect:
Prepared by the present invention presses against the piezo-electric damping material maximum loss factor (tan δ max) >=0.7 as conductive channel to gather arsenic, effective damping temperature range (Δ T0.7) >=40 ℃, in 30 ℃ of temperature, range of frequency 1Hz～1000Hz dissipation factor (tan α) >=0.5, it is 20 ℃～100 ℃ in the temperature range of range of frequency 1Hz～1000Hz dissipation factor (tan α) >=0.3.
Embodiment
Explanation the present invention that can be detailed by the following examples, discloses object of the present invention and is intended to protect all technological improvements in the scope of the invention.
Embodiment 1:
Press against/piezoelectric ceramic powder composite material of poly-arsenic composition and mass fraction are 100 parts of magnesium niobium lead zirconate titanate type piezoelectric ceramics, and arsenic is pressed against 30 parts of monomers, 15 parts of hydrochloric acid.
First in there-necked flask, add magnesium niobium lead zirconate titanate type piezoelectric ceramic powder, then there-necked flask is fixed on the iron stand with whipping appts, flask approximately 3/4ths parts are immersed in the water bath with thermostatic control of 80 ℃, turn on agitator, in there-necked flask, add distilled water again, the material being bonded in flask walls is poured to there-necked flask bottom, itself and distilled water are mixed.After 80 ℃ of constant temperature 10min of water-bath, under whipped state, first arsenic is pressed against gradually and joined in there-necked flask, then hydrochloric acid is joined in there-necked flask gradually, under strong stirring, constant temperature water bath reaction is carried out 24 hours.After having reacted, close water-bath, after question response thing is cooling, filter with vacuum filtration device, then use absolute ethanol washing, wash 4 times, the black powder obtaining is encased in culture dish, under state of nature, ethanol is volatilized gradually, after 24 hours, grind black powder with mortar it is scatter, again material is put in the baking oven of 100 ℃ dry 3 hours, completed the preparation of poly-press against/piezoelectric ceramic powder composite material of arsenic.
Piezo-electric damping material composition and mass fraction are: 100 parts of chlorosulfonated polyethylenes, 1 part of accelerant disulfide dibenzo thiophene DM, 1 part, sulphur, 1 part of antioxidant 4010NA, 50 parts, mica powder 80 order, 10 parts of epoxy resin E-51,100 parts of press against/piezoelectric ceramic powders of poly-arsenic.
In mill, chlorosulfonated polyethylene is plasticated, add anti-aging agent, mica powder, poly-press against/piezoelectric ceramic powder of arsenic, epoxy resin, promotor, sulphur, mixing even, sulfidization molding on vulcanizing press, pressure 12MPa, 160 ℃ of temperature, curing time 40min.
Conductive silver glue is stirred, with the even sizing material two sides of brushing at sulfidization molding of hairbrush, be dry 3h in the loft drier of 100 ℃ in temperature, after cooling in room temperature environment, putting into high voltage direct current oil bath device polarizes again, strength of electric field is 1kv/mm, and polarization 30min, completes the preparation of piezo-electric damping material.
Embodiment 2:
Press against/piezoelectric ceramic powder composite material of poly-arsenic composition and mass fraction are 100 parts of modification magnesium niobium lead zirconate titanate type piezoelectric ceramics, and arsenic is pressed against 45 parts of monomers, 25 parts of hydrochloric acid.
First in there-necked flask, add modification magnesium niobium lead zirconate titanate type piezoelectric ceramic powder, then there-necked flask is fixed on the iron stand with whipping appts, flask approximately 3/4ths parts are immersed in the water bath with thermostatic control of 70 ℃, turn on agitator, in there-necked flask, add distilled water again, the material being bonded in flask walls is poured to there-necked flask bottom, itself and distilled water are mixed.After 70 ℃ of constant temperature 20min of water-bath, under whipped state, first arsenic is pressed against gradually and joined in there-necked flask, then hydrochloric acid is joined in there-necked flask gradually, under strong stirring, constant temperature water bath reaction is carried out 28 hours.After having reacted, close water-bath, after question response thing is cooling, filter with vacuum filtration device, then use absolute ethanol washing, wash 3 times, the black powder obtaining is encased in culture dish, under state of nature, ethanol is volatilized gradually, after 28 hours, grind black powder with mortar it is scatter, again material is put in the baking oven of 110 ℃ dry 2 hours, completed the preparation of poly-press against/piezoelectric ceramic powder composite material of arsenic.
Piezo-electric damping material composition and mass fraction are: 100 parts of paracrils, 3 parts of vulkacit Ds, 3 parts, sulphur, 2 parts of antioxidant A W, 150 parts, mica powder 200 order, 50 parts of E-44,500 parts of press against/piezoelectric ceramic powders of poly-arsenic.
In mill, paracril is plasticated, add anti-aging agent, mica powder, poly-press against/piezoelectric ceramic powder of arsenic, epoxy resin, promotor, sulphur, mixing even, sulfidization molding on vulcanizing press, pressure 10MPa, 150 ℃ of temperature, curing time 20min.
Conductive silver glue is stirred, with the even sizing material two sides of brushing at sulfidization molding of hairbrush, be dry 2h in the loft drier of 120 ℃ in temperature, after cooling in room temperature environment, putting into high voltage direct current oil bath device polarizes again, strength of electric field is 3kv/mm, and polarization 20min, completes the preparation of piezo-electric damping material.
Embodiment 3:
Press against/piezoelectric ceramic powder composite material of poly-arsenic composition and mass fraction are 100 parts of Pb-based lanthanumdoped zirconate titanates type piezoelectric ceramics, and arsenic is pressed against 60 parts of monomers, 30 parts of hydrochloric acid.
First in there-necked flask, add Pb-based lanthanumdoped zirconate titanates type piezoelectric ceramics, then there-necked flask is fixed on the iron stand with whipping appts, flask approximately 3/4ths parts are immersed in the water bath with thermostatic control of 75 ℃, turn on agitator, in there-necked flask, add distilled water again, the material being bonded in flask walls is poured to there-necked flask bottom, itself and distilled water are mixed.After 75 ℃ of constant temperature 15min of water-bath, under whipped state, first arsenic is pressed against gradually and joined in there-necked flask, then hydrochloric acid is joined in there-necked flask gradually, under strong stirring, constant temperature water bath reaction is carried out 26 hours.After having reacted, close water-bath, after question response thing is cooling, filter with vacuum filtration device, then use absolute ethanol washing, wash 4 times, the black powder obtaining is encased in culture dish, under state of nature, ethanol is volatilized gradually, after 26 hours, grind black powder with mortar it is scatter, again material is put in the baking oven of 105 ℃ dry 2.5 hours, completed the preparation of poly-press against/piezoelectric ceramic powder composite material of arsenic.
Piezo-electric damping material composition and mass fraction are: 100 parts of urethaness, 5 parts of Vulcanization accelerator TMTDs, 5 parts, sulphur, 3 parts of antioxidant Ds, 200 parts, mica powder 325 order, 50 parts of E-44,50 parts of E-51,1000 parts of press against/piezoelectric ceramic powders of poly-arsenic.
In mill, urethanes is plasticated, add anti-aging agent, mica powder, poly-press against/piezoelectric ceramic powder of arsenic, epoxy resin, promotor, sulphur, mixing even, sulfidization molding on vulcanizing press, pressure 11MPa, 155 ℃ of temperature, curing time 30min.
Conductive silver glue is stirred, with the even sizing material two sides of brushing at sulfidization molding of hairbrush, be dry 2.5h in the loft drier of 110 ℃ in temperature, after cooling in room temperature environment, putting into high voltage direct current oil bath device polarizes again, strength of electric field is 2kv/mm, and polarization 25min, completes the preparation of piezo-electric damping material.
Embodiment 4:
Press against/piezoelectric ceramic powder composite material of poly-arsenic composition and mass fraction are 100 parts of Pb-based lanthanumdoped zirconate titanates type piezoelectric ceramics, and arsenic is pressed against 60 parts of monomers, 30 parts of ferric chloride Solutions.
First in there-necked flask, add Pb-based lanthanumdoped zirconate titanates type piezoelectric ceramics, then there-necked flask is fixed on the iron stand with whipping appts, flask approximately 3/4ths parts are immersed in the water bath with thermostatic control of 80 ℃, turn on agitator, in there-necked flask, add distilled water again, the material being bonded in flask walls is poured to there-necked flask bottom, itself and distilled water are mixed.After 80 ℃ of constant temperature 20min of water-bath, under whipped state, first arsenic is pressed against gradually and joined in there-necked flask, then hydrochloric acid is joined in there-necked flask gradually, under strong stirring, constant temperature water bath reaction is carried out 24 hours.After having reacted, close water-bath, after question response thing is cooling, filter with vacuum filtration device, then use absolute ethanol washing, wash 4 times, the black powder obtaining is encased in culture dish, under state of nature, ethanol is volatilized gradually, after 24 hours, grind black powder with mortar it is scatter, again material is put in the baking oven of 120 ℃ dry 2 hours, completed the preparation of poly-press against/piezoelectric ceramic powder composite material of arsenic.
Piezo-electric damping material composition and mass fraction are: 100 parts of natural rubber rubber, 2 parts of altaxs, 1 part of vulkacit D, 5 parts, sulphur, 3 parts of antioxidant Ds, 100 parts, mica powder 200 order, 500 parts, mica powder 325 order, 50 parts of E-44,50 parts of E-51,1000 parts of press against/piezoelectric ceramic powders of poly-arsenic.
In mill, natural rubber is plasticated, add anti-aging agent, mica powder, poly-press against/piezoelectric ceramic powder of arsenic, epoxy resin, promotor, sulphur, mixing even, sulfidization molding on vulcanizing press, pressure 10MPa, 150 ℃ of temperature, curing time 20min.
Conductive silver glue is stirred, with the even sizing material two sides of brushing at sulfidization molding of hairbrush, be dry 2h in the loft drier of 110 ℃ in temperature, after cooling in room temperature environment, putting into high voltage direct current oil bath device polarizes again, strength of electric field is 3kv/mm, and polarization 30min, completes the preparation of piezo-electric damping material.
Embodiment 1～4 performance formula test result is as shown in table 1.
Table 1 embodiment 1～4 performance formula test result
Part not in the detailed description of the invention is prior art.
Claims (9)
1. a poly-arsenic is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: described piezo-electric damping material component be by weight: 100 parts of rubber, 1～5 part of promotor, 1～5 part, sulphur, 1～3 part, anti-aging agent, 50～200 parts of mica powders, 10～100 parts of epoxy resin, 100～1000 parts of press against/piezoelectric ceramic powder composite materials of poly-arsenic; Wherein said press against/piezo-electric ceramic composite material of poly-arsenic component be by weight: 100 parts of piezoelectric ceramic powders, arsenic is pressed against 30～60 parts of monomers, 15～30 parts of initiators; Described piezoelectric ceramic powder is the one in magnesium niobium lead zirconate titanate type piezoelectric ceramics, Pb-based lanthanumdoped zirconate titanates type piezoelectric ceramics or modification magnesium niobium lead zirconate titanate type piezoelectric ceramics.
2. poly-arsenic as claimed in claim 1 is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: described rubber is the one in paracril, natural rubber, chlorosulfonated polyethylene, urethanes.
3. poly-arsenic as claimed in claim 1 is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: described promotor is one or both in dibenzothiazyl disulfide DM, vulkacit D D and tetramethyl-dithio thiuram TMTD.
4. poly-arsenic as claimed in claim 1 is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: described anti-aging agent is the one in antioxidant 4010NA, antioxidant A W, antioxidant D.
5. poly-arsenic as claimed in claim 1 is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: described mica powder is one or both in 80 orders, 200 orders and 325 orders.
6. poly-arsenic as claimed in claim 1 is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: described epoxy resin is one or both in E-51, E-44.
7. poly-arsenic as claimed in claim 1 is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: the particle diameter of described piezoelectric ceramic powder is 1-10um.
8. a preparation method for press against/piezoelectric ceramic powder composite material of poly-arsenic as claimed in claim 1, uses chemical oxidation situ aggregation method, it is characterized in that: comprise the following steps:
(1) obtain solution: first add piezoelectric ceramic powder in there-necked flask, be immersed in the water bath with thermostatic control of 70 ℃～80 ℃, add distilled water to mix, after constant temperature 10～20min, under whipped state, add successively that arsenic is pressed against, hydrochloric acid in there-necked flask, stir and obtain black mixing solutions;
(2) isothermal reaction: constant temperature water bath reaction is carried out 24 ~ 28 hours;
(3) aftertreatment: after having reacted, close water-bath, after reactant is cooling, filter with vacuum filtration device, then use absolute ethanol washing 3 ~ 4 times, obtain black powder; The black powder obtaining is encased in culture dish, and ethanol is volatilized gradually; Then grind black powder with mortar it is scatter, then material is put in the baking oven of 100 ℃～110 ℃ dry 2～3 hours.
9. poly-arsenic as claimed in claim 1 is pressed against the piezo-electric damping material into conductive channel, it is characterized in that: comprise the following steps:
(1) preparation of blank: by formula, after rubber is plasticated in mill, add poly-press against/piezoelectric ceramic powder composite material of arsenic, epoxy resin, mica powder, anti-aging agent, promotor, sulphur, mixing even;
(2) sulfuration: be 10～12MPa by blank pressure in metal die, temperature is 150～160 ℃, and curing time is that under 20～40min condition, sulfidization molding becomes sizing material;
(3) polarization: conductive silver glue is stirred, brush on the sizing material two sides of sulfidization molding, at 100～120 ℃ of dry 2～3h of temperature, the cooling rear electrode processing of room temperature, can obtain piezo-electric damping material of the present invention.
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| CN201410102861.0A CN103881253B (en) | 2014-03-19 | 2014-03-19 | A kind of poly- arsenic presses against piezo-electric damping material and preparation method for conductive channel |
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| CN201410102861.0A CN103881253B (en) | 2014-03-19 | 2014-03-19 | A kind of poly- arsenic presses against piezo-electric damping material and preparation method for conductive channel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108586846A (en) * | 2018-04-28 | 2018-09-28 | 武汉工程大学 | A kind of low frequency absorption rubber composite material and preparation method thereof based on cavity structure |
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