CN106750656B - A kind of barium titanate/rubber piezo-electricity composite material and preparation method thereof for low frequency absorption - Google Patents
A kind of barium titanate/rubber piezo-electricity composite material and preparation method thereof for low frequency absorption Download PDFInfo
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Abstract
The invention belongs to low frequency absorption Material Fields, and in particular to a kind of barium titanate/rubber piezo-electricity composite material and preparation method thereof for low frequency absorption.The present invention first pre-processes barium titanate ceramics powder, then it is function phase using piezoelectric ceramics, conductive black is conductive phase, nitrile rubber for matrix, the principle being combined with bulk effect using piezoelectric effect, the barium titanate for low frequency absorption/rubber piezo-electricity composite material is prepared, the damping temperature domain of the barium titanate/rubber piezo-electricity composite material is wider, and storage modulus is higher；Based on piezoelectric effect and bulk effect principle, the barium titanate/rubber piezo-electricity composite material can obtain preferable effect of low-frequency sound absorption in the case where thickness is smaller.
Description
Technical field
The invention belongs to low frequency absorption Material Fields, and in particular to a kind of barium titanate/rubber piezoelectricity for low frequency absorption
Composite material and preparation method.
Background technology
The development of modern industry makes noise problem be on the rise, and long-time contact noise will produce bad work to body
With can also be had an impact to vision, respiratory system, human immune system and development of fetus, the research system for the damping material that absorbs sound
It is standby to be particularly important.Traditional sound-absorbing material includes mainly foam class, fiber-like, resonance class and composite material class, undulation degree
Material is preferable in medium-high frequency sound absorption, but low frequency absorption is poor；The foamed materials low frequency absorption such as polyurethane is poor and intensity is relatively low；Resonance
Class material needs special construction, and sound absorption frequency range is relatively narrow, and limitation is larger and material thickness is larger；And composite processing
It is modified convenient, different use environments can be met.Wherein piezo-electricity composite material is a kind of more novel sound absorption vibration damping composite wood
Material, sound absorption frequency are smaller to temperature dependency.
The crystalline material that can occur voltage between end face when being acted on by external mechanical force is known as piezoelectric material.Utilize piezoelectricity
These characteristics of material can realize mechanical oscillation (sound wave) and the mutual conversion of electric current.Piezoelectric material performance largely depends on
In the synthesis of piezo-electric crystal.The synthetic method of piezo-electric crystal can generally be divided into solid phase method, liquid phase method and vapor phase method.Solid phase method
Including traditional reaction method, high-energy ball milling method, combustion method etc.；Liquid phase method includes solution-gel method, hydro-thermal method (hot solvent method), grass
Hydrochlorate method, coprecipitation etc.；Vapor phase method includes physical vapour deposition (PVD) and chemical vapor deposition.Liquid phase method is because of its reaction condition temperature
With crystallinity preferably, chemical composition stability the advantages that and be widely used in the preparation of piezo-electric crystal.
According to the packing property and external design structure adulterated into rubber, can design multiple damping mechanism (matrix and
Energy loss caused by the interior friction of fibre reinforced materials, mesomerism, interface friction heat, viscoplasticity damping etc.), it increases
The strong compound use value as vibration and noise reducing material.Traditional sound absorption such as rigidifying of decoupling, vibration isolation and structure is different to subtract
Method of slight, piezo-electricity composite material inside have a variety of energy conversion machine systems, include the conversion (piezo-electric damping of mechanical energy and electric energy
Material), the conversion (reversible hydrogen bond energy consumption damping material) of mechanical energy and chemical energy, the conversion (rare earth permanent magnet of mechanical energy and magnetic energy
Damping material) etc., it can develop novel sound absorption damping material using these mechanism.When sound wave or the vibration mechanical energy of other forms
When being applied to piezo-electricity composite material surface, electric energy is translated by direct piezoelectric effect, in the piezoelectric unit of composite material
Interior generation alternating voltage, when composite inner resistance is excessive or resistance is too small, the electric energy of generation cannot conduct dissipation immediately,
Since inverse piezoelectric effect can be again converted to vibrational energy.In this way, positive inverse piezoelectric effect repeat function, vibrational energy persistently decline
Subtract, finally dissipated in the form of thermal energy, to play the effect of vibration and noise reducing.
Invention content
The present invention is in view of the deficiencies of the prior art, and it is an object of the present invention to provide a kind of barium titanate/rubber pressure for low frequency absorption
Composite and preparation method thereof.
For achieving the above object, the technical solution adopted by the present invention is：
A kind of preparation method of barium titanate/rubber piezo-electricity composite material for low frequency absorption, includes the following steps：
(1) pretreatment of barium titanate ceramics powder：First by barium titanate ceramics powder be put into ball milling 5 in ball mill~
15min obtains barium titanate ceramics powder, then barium titanate ceramics powder and modifying agent is placed in high-speed mixer, with 1200
~1500r/min 10~30min of high-speed stirred obtain pretreated barium titanate ceramics powder, spare after dry；
(2) rubber matrix raw material is weighed according to the following formulation：100 parts by weight of nitrile rubber, 3~8 parts by weight of ZnO, stearic acid
0.5~3 parts by weight of zinc, 0.5~2 parts by weight of antioxidant 4010,1~3 parts by weight of sulphur, promote 0.5~3 parts by weight of stearic acid
0.5~2 parts by weight of agent DM, 0.5~2 parts by weight of accelerant CZ；After weighing pretreatment obtained by conductive black and step (1) simultaneously
Barium carbonate powder；
(3) sequentially added in mixer or open mill zinc oxide, stearic acid, zinc stearate, anti-aging agent, altax,
Accelerant CZ, pretreated barium titanate ceramics powder, conductive black and sulphur, at a temperature of 40~80 DEG C be kneaded 10~
40min obtains rubber compound, and rubber compound obtains the barium titanate for low frequency absorption/rubber piezo-electricity composite material after vulcanization.
In said program, step (1) described modifying agent is silane coupling agent, titanate coupling agent, stearic acid or tristearin
Hydrochlorate.
In said program, the mass ratio of pretreated barium titanate ceramic powder and modifying agent described in step (1) is
100:1~6.
In said program, the volume of step (2) described conductive black accounts for the 2%~10% of rubber matrix raw material total volume,
The volume of the pretreated barium carbonate powder accounts for the 10%~60% of rubber matrix raw material total volume.
In said program, the temperature of step (3) described vulcanization is 155~175 DEG C, and the time is 15~30min.
In said program, the pressure of step (3) described vulcanization is 10~20MPa.
The barium titanate for low frequency absorption/rubber piezo-electricity composite material that above-mentioned preparation method is prepared.
Beneficial effects of the present invention：The present invention first pre-processes barium titanate ceramics powder, then with piezoelectric ceramics
For function phase, conductive black be conductive phase, nitrile rubber is matrix, the principle being combined with bulk effect using piezoelectric effect,
The barium titanate for low frequency absorption/rubber piezo-electricity composite material, the resistance of the barium titanate/rubber piezo-electricity composite material is prepared
Buddhist nun's temperature range is wider, and storage modulus is higher；Based on piezoelectric effect and bulk effect principle, the barium titanate/rubber Piezoelectric anisotropy material
Material can obtain preferable effect of low-frequency sound absorption in the case where thickness is smaller.
Description of the drawings
Fig. 1 is the damping capacity of 2mm piezo-electricity composite material products under different temperatures in embodiment 3.
Fig. 2 is the damping capacity of 2mm piezo-electricity composite material products under different frequency in embodiment 3.
Fig. 3 is the low frequency absorption performance of 2mm piezo-electricity composite material products in embodiment 3.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
A kind of barium titanate/rubber piezo-electricity composite material for low frequency absorption is prepared via a method which to obtain：
(1) barium titanate ceramics powder pre-processes：Barium titanate ceramics powder is put into ball milling 5min in ball mill；Using silane
Coupling agent is modifying agent, and dosage is the 2% of barium titanate ceramics powder quality；Barium titanate ceramics powder after ball milling is tried with modified
Agent is placed in high-speed mixer, and 20min is stirred with high speed 1200r/min, obtains pretreated barium titanate ceramics powder, and drying is standby
With；
(2) rubber matrix raw material is weighed by formula as below：100 parts by weight of nitrile rubber, 4 parts by weight of ZnO, zinc stearate 1
Parts by weight, 1 parts by weight of stearic acid, 0.8 parts by weight of antioxidant 4010,1 parts by weight of sulphur, 0.8 parts by weight of altax promote
0.8 parts by weight of agent CZ；Weigh conductive black simultaneously (volume of conductive black is the 4% of rubber matrix raw material total volume)；Metatitanic acid
Titanate ceramics powder (volume of barium titanate ceramics powder is the 30% of rubber matrix raw material total volume)；
(3) sequentially added in mixer or open mill zinc oxide, stearic acid, zinc stearate, anti-aging agent, altax,
Accelerant CZ, barium titanate ceramics powder, conductive black and sulphur are kneaded 20min at 80 DEG C or less and obtain rubber compound, and rubber compound exists
160 DEG C, vulcanize 25min under the conditions of 15MPa, obtain the barium titanate for low frequency absorption/rubber piezo-electricity composite material.
Effect assessment：Thickness is the composite product of 2mm, and under low frequency environments, averagely damping is under different frequency
For average damped coefficient 0.74 or so, maximum low frequency acoustic absorptivity is 0.25 to number between 0.2 or so, -20~0 DEG C.
Embodiment 2
A kind of barium titanate/rubber piezo-electricity composite material for low frequency absorption is prepared via a method which to obtain：
(1) barium titanate ceramics powder pre-processes：Barium titanate ceramics powder is put into ball milling 8min in ball mill；Using silane
Coupling agent is modifying agent, and dosage is the 3% of barium titanate ceramics powder quality；Barium titanate ceramics powder after ball milling is tried with modified
Agent is placed in high-speed mixer, and 25min is stirred with high speed 1300r/min, obtains pretreated barium titanate ceramics powder, and drying is standby
With；
(2) rubber matrix raw material is weighed by formula as below：100 parts by weight of nitrile rubber, 4 parts by weight of ZnO, zinc stearate 1
Parts by weight, 1 parts by weight of stearic acid, 0.8 parts by weight of antioxidant 4010,1 parts by weight of sulphur, 0.8 parts by weight of altax promote
0.8 parts by weight of agent CZ；Weigh conductive black simultaneously (volume of conductive black is the 8% of rubber matrix raw material total volume)；Metatitanic acid
Titanate ceramics powder (volume of barium titanate ceramics powder is the 40% of rubber matrix raw material total volume)；
(3) sequentially added in mixer or open mill zinc oxide, stearic acid, zinc stearate, anti-aging agent, altax,
Accelerant CZ, barium titanate ceramics powder, conductive black and sulphur are kneaded 20min at 60 DEG C or less and obtain rubber compound, and rubber compound exists
170 DEG C, vulcanize 25min under the conditions of 10MPa, obtain the barium titanate for low frequency absorption/rubber piezo-electricity composite material.
Effect assessment：Thickness is the composite product of 2mm, and under low frequency environments, averagely damping is under different frequency
For average damped coefficient 0.76 or so, maximum low frequency acoustic absorptivity is 0.255 to number between 0.2 or so, -20~0 DEG C.
Embodiment 3
A kind of barium titanate/rubber piezo-electricity composite material for low frequency absorption is prepared via a method which to obtain：
(1) barium titanate ceramics powder pre-processes：Barium titanate ceramics powder is put into ball milling 10min in ball mill；Using silicon
Alkane coupling agent is modifying agent, and dosage is the 5% of barium titanate ceramics powder quality；By after ball milling barium titanate ceramics powder and modification
Reagent is placed in high-speed mixer, is stirred 20min with high speed 1400r/min, is obtained pretreated barium titanate ceramics powder, dry
It is spare；
(2) rubber matrix raw material is weighed by formula as below：100 parts by weight of nitrile rubber, 4 parts by weight of ZnO, zinc stearate 1
Parts by weight, 1 parts by weight of stearic acid, 0.8 parts by weight of antioxidant 4010,1 parts by weight of sulphur, 0.8 parts by weight of altax promote
0.8 parts by weight of agent CZ；Weigh conductive black simultaneously (volume of conductive black is the 6% of rubber matrix raw material total volume)；Metatitanic acid
Titanate ceramics powder (volume of barium titanate ceramics powder is the 50% of rubber matrix raw material total volume)；
(3) sequentially added in mixer or open mill zinc oxide, stearic acid, zinc stearate, anti-aging agent, altax,
Accelerant CZ, barium titanate ceramics powder, conductive black and sulphur are kneaded 30min at 70 DEG C or less and obtain rubber compound, and rubber compound exists
170 DEG C, vulcanize 25min under the conditions of 10MPa, obtain the barium titanate for low frequency absorption/rubber piezo-electricity composite material.
Effect assessment：Thickness is the composite product of 2mm, damping capacity test result such as Fig. 1 under different temperatures
Shown, test results are shown in figure 2 for the damping capacity under different frequency, and low frequency absorption the performance test results are as shown in Figure 3.From figure
1~3 can be seen that：Under low frequency environments, average damped coefficient averagely hinders between 0.3 or so, -20~0 DEG C under different frequency
For Buddhist nun's coefficient 0.8 or so, maximum low frequency acoustic absorptivity is 0.32.
Embodiment 4
A kind of barium titanate/rubber piezo-electricity composite material for low frequency absorption is prepared via a method which to obtain：
(1) barium titanate ceramics powder pre-processes：Barium titanate ceramics powder is put into ball milling 10min in ball mill；Using silicon
Alkane coupling agent is modifying agent, and dosage is the 3% of barium titanate ceramics powder quality；By after ball milling barium titanate ceramics powder and modification
Reagent is placed in high-speed mixer, is stirred 20min with high speed 1300r/min, is obtained pretreated barium titanate ceramics powder, dry
It is spare；
(2) rubber matrix raw material is weighed by formula as below：100 parts by weight of nitrile rubber, 4 parts by weight of ZnO, zinc stearate 1
Parts by weight, 1 parts by weight of stearic acid, 0.8 parts by weight of antioxidant 4010,1 parts by weight of sulphur, 0.8 parts by weight of altax promote
0.8 parts by weight of agent CZ；Weigh conductive black simultaneously (volume of conductive black is the 2% of rubber matrix raw material total volume)；Metatitanic acid
Titanate ceramics powder (volume of barium titanate ceramics powder is the 40% of rubber matrix raw material total volume)；
(3) sequentially added in mixer or open mill zinc oxide, stearic acid, zinc stearate, anti-aging agent, altax,
Accelerant CZ, barium titanate ceramics powder, conductive black and sulphur are kneaded 30min at 60 DEG C or less and obtain rubber compound, and rubber compound exists
175 DEG C, vulcanize 15min under the conditions of 10MPa, obtain the barium titanate for low frequency absorption/rubber piezo-electricity composite material.
Effect assessment：Thickness is the composite product of 2mm.Under low frequency environments, averagely damping is under different frequency
For average damped coefficient 0.75 or so, maximum low frequency acoustic absorptivity is 0.25 to number between 0.21 or so, -20~0 DEG C.
Embodiment 5
A kind of barium titanate/rubber piezo-electricity composite material for low frequency absorption is prepared via a method which to obtain：
(1) barium titanate ceramics powder pre-processes：Barium titanate ceramics powder is put into ball milling 10min in ball mill；Using silicon
Alkane coupling agent is modifying agent, and dosage is the 5% of barium titanate ceramics powder quality；By after ball milling barium titanate ceramics powder and modification
Reagent is placed in high-speed mixer, is stirred 30min with high speed 1500r/min, is obtained pretreated barium titanate ceramics powder, dry
It is spare；
(2) rubber matrix raw material is weighed by formula as below：100 parts by weight of nitrile rubber, 4 parts by weight of ZnO, zinc stearate 1
Parts by weight, 1 parts by weight of stearic acid, 0.8 parts by weight of antioxidant 4010,1 parts by weight of sulphur, 0.8 parts by weight of altax promote
0.8 parts by weight of agent CZ；Weigh conductive black simultaneously (volume of conductive black is the 10% of rubber matrix raw material total volume)；Titanium
Sour titanate ceramics powder (volume of barium titanate ceramics powder is the 60% of rubber matrix raw material total volume)；
(3) sequentially added in mixer or open mill zinc oxide, stearic acid, zinc stearate, anti-aging agent, altax,
Accelerant CZ, barium titanate ceramics powder, conductive black and sulphur are kneaded 40min at 60 DEG C or less and obtain rubber compound, and rubber compound exists
170 DEG C, vulcanize 25min under the conditions of 15MPa, obtain the barium titanate for low frequency absorption/rubber piezo-electricity composite material.
Effect assessment：Thickness is the composite product of 2mm.Under low frequency environments, averagely damping is under different frequency
For average damped coefficient 0.85 or so, maximum low frequency acoustic absorptivity is 0.11 to number between 0.3 or so, -20~0 DEG C.
Obviously, above-described embodiment be only intended to clearly illustrate made by example, and not limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection domain of the invention.
Claims (4)
1. a kind of preparation method of barium titanate/rubber piezo-electricity composite material for low frequency absorption, which is characterized in that including as follows
Step：
（1）The pretreatment of barium titanate ceramics powder：Barium titanate ceramics powder 5 ~ 15min of ball milling in ball mill is put into first to obtain
Then barium titanate ceramics powder and modifying agent are placed in high-speed mixer by barium titanate ceramics powder, with 1200 ~ 1500 r/
10 ~ 30 min of min high-speed stirreds obtains pretreated barium titanate ceramics powder, spare after dry；The modifying agent is silicon
Alkane coupling agent, titanate coupling agent, stearic acid or stearate；
（2）Rubber matrix raw material is weighed according to the following formulation：100 parts by weight of nitrile rubber, 3 ~ 8 parts by weight of ZnO, zinc stearate
0.5 ~ 3 parts by weight, 0.5 ~ 3 parts by weight of stearic acid, 0.5 ~ 2 parts by weight of antioxidant 4010,1 ~ 3 parts by weight of sulphur, altax
0.5 ~ 2 parts by weight, 0.5 ~ 2 parts by weight of accelerant CZ；Weigh conductive black and step simultaneously（1）The pretreated metatitanic acid of gained
Titanate ceramics powder；
（3）Nitrile rubber, zinc oxide, stearic acid, zinc stearate, anti-aging agent, promotion are sequentially added in mixer or open mill
Agent DM, accelerant CZ, pretreated barium titanate ceramic powder, conductive black and sulphur, at a temperature of 40 ~ 80 DEG C be kneaded 10 ~
40min obtains rubber compound, and rubber compound obtains the barium titanate for low frequency absorption/rubber piezo-electricity composite material after vulcanization, described
The temperature of vulcanization is 155 ~ 175 DEG C, and the time is 15 ~ 30min, and pressure is 10 ~ 20MPa.
2. preparation method according to claim 1, which is characterized in that step（1）The barium titanate ceramics powder and modification
The mass ratio of reagent is 100:1~6.
3. preparation method according to claim 1, which is characterized in that step（2）The volume of the conductive black accounts for rubber
The volume of the 2% ~ 10% of matrix material total volume, the pretreated barium carbonate powder accounts for rubber matrix raw material total volume
10%~60%。
4. the barium titanate for low frequency absorption/rubber Piezoelectric anisotropy that any preparation method of claim 1 ~ 3 is prepared
Material.
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| CN107283950A (en) * | 2017-06-30 | 2017-10-24 | 武汉工程大学 | It is a kind of for layer structure composite of low frequency absorption and preparation method thereof |
| CN108384127A (en) * | 2018-03-12 | 2018-08-10 | 衡水中铁建环保工程有限公司 | A kind of preparation method of open cell type rubber acoustic board |
| CN108641140B (en) * | 2018-04-28 | 2020-11-27 | 武汉工程大学 | Rare earth oxide/nitrile rubber-polyurethane foam double-layer composite material for low-frequency sound absorption and preparation method thereof |
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| JP2002121327A (en) * | 2000-10-16 | 2002-04-23 | Sumitomo Rubber Ind Ltd | Tread rubber composition and manufacturing method therefor |
| CN101974181B (en) * | 2010-11-17 | 2013-07-10 | 武汉工程大学 | Method for preparing rare-earth oxide/rubber composite material for low-frequency sound absorption |
| CN106009104A (en) * | 2016-06-26 | 2016-10-12 | 青岛海蓝海洋复合功能材料科技有限公司 | Magnetic rubber material with stability |
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2016
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