CN109166960A - A kind of preparation method of fiber base flexible piezoelectric sensors - Google Patents

A kind of preparation method of fiber base flexible piezoelectric sensors Download PDF

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CN109166960A
CN109166960A CN201810968664.5A CN201810968664A CN109166960A CN 109166960 A CN109166960 A CN 109166960A CN 201810968664 A CN201810968664 A CN 201810968664A CN 109166960 A CN109166960 A CN 109166960A
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preparation
fiber base
piezoelectric sensors
samarium
solution
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万军民
吕思佳
胡智文
王秉
彭志勤
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Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10NELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00Piezoelectric or electrostrictive devices
    • H10N30/01Manufacture or treatment
    • H10N30/09Forming piezoelectric or electrostrictive materials
    • H10N30/092Forming composite materials
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/003Titanates
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/56Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of cyclic compounds with one carbon-to-carbon double bond in the side chain
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10NELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00Piezoelectric or electrostrictive devices
    • H10N30/01Manufacture or treatment
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10NELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00Piezoelectric or electrostrictive devices
    • H10N30/01Manufacture or treatment
    • H10N30/09Forming piezoelectric or electrostrictive materials
    • H10N30/093Forming inorganic materials

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Abstract

The present invention relates to sensor fields, disclose a kind of preparation method of fiber base flexible piezoelectric sensors, the present invention passes through nanocrystalline with samarium doping lead titanates, modified lead titanate piezoelectric ceramic, the Curie temperature for mixing the modified lead titanate piezoelectric ceramics of samarium is higher, and mechanical-electric coupling anisotropy is big, more suitable for the various energy converters to work under production high temperature, and by its ball milling at nano particle, enlarged contact areas.Then surface functionalization is carried out with amino, it is ensured that with the maleic anhydride molecule covalent coupling in polymer substrate.Compared with unmodified nanoparticles, it can be uniformly distributed in polymer composites, and improve piezo-electric generating.A fiber base flexible piezoelectric sensors finally are obtained by wet spinning, improve flexible and stability, and the scope of application that its stitchability expands sensor has more excellent detection performance compared with traditional sensors.Inventive sensor is flexible, can be applied to medical biological monitoring, the fields such as environment and the monitoring of hygiene.

Description

A kind of preparation method of fiber base flexible piezoelectric sensors
Technical field
The present invention relates to sensor field more particularly to a kind of preparation methods of fiber base flexible piezoelectric sensors.
Background technique
Sensor is that mankind itself finds out the various sensory informations of nature, can be turned to unlike signal and perception information Turn to can digitize, intelligentized important devices.During human civilization rapid development of information technology, sensor is played Increasingly heavier effect is mankind's exploration outfield, while being also that the mankind understand real world, observes the important of peripheral information One of means.Sensor be it is a kind of the non-electrical signal such as electricity, light, temperature and chemical action can be converted into electrical signal can The component of regulation.
In recent years, as the fast development of flexible wearable formula electronic product, flexible sensor and flexible energy-storage travelling wave tube draw Extensive concern is played.The important component of flexible sensor and flexible energy-storage travelling wave tube as wearable electronic, in people There is huge application prospect in the fields such as body motion detection, personalized health monitoring and intelligent human-machine interaction.Wherein, flexible to pass Sensor should have both high sensitivity, wide detection range, high flexibility and high stability, and flexible energy-storage travelling wave tube should have excellent electrification Learn performance, good mechanical flexibility etc..So far, preparing these ideal flexible devices is still a no small challenge.It is logical It crosses and material select and is expected to obtain the flexible device of excellent combination property using new technology of preparing and mentality of designing.It leads Electric macromolecular fibre base flexible piezoelectric sensors because its flexibility is good, light weight, foldable bending, can weave, it is at low cost and The features such as large specific surface area, has become one of the important directions of flexible device research
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of preparation methods of fiber base flexible piezoelectric sensors. Preparation method of the present invention is nanocrystalline by preparing samarium doping lead titanates, and modified tradition lead titanate piezoelectric ceramics makes its Curie temperature It improves, lattice anisotropy becomes larger, and with ball mill ball milling at nano particle, then with amido modified samarium doping lead titanates nanometer Particle realizes surface functionalization with covalent coupling, finally obtains a kind of fiber base flexible piezoelectric sensors by wet spinning, with Traditional sensors, which are compared, has more excellent detection performance.
The specific technical proposal of the invention is: a kind of preparation method of fiber base flexible piezoelectric sensors, including walk as follows It is rapid:
(1) the nanocrystalline preparation of samarium doping lead titanates: deionized water is added in butyl titanate under agitation, is suspended After liquid, the aqueous solution of lead acetate, samarium trichloride, sodium hydroxide is sequentially added under agitation, last constant volume to 250-300ml, Obtain mixed solution;Mixed solution is added to oil bath heating in reaction kettle and is stirred 4-5 minutes, 8-10h is kept the temperature after heating;To After the reaction was completed, room temperature is naturally cooled to, product is taken out and impregnates, makes soluble ion that sufficiently exchange occur, filtering and washing removes Soluble ion, the then dry 6-8h at 80-100 DEG C, being cooled to room temperature, to obtain samarium doping lead titanates nanocrystalline.
Lead titanates is that calcium is admired the ferroelectric material of mine structure, and curie point is high, and relative dielectric constant is small, and pyroelectricity constant is big, Laterally and longitudinally there is very big anisotropy between electromechanical coupling factor.But since the crystal boundary energy that lead titanates becomes ceramics is high, four Square coercive field is big, and lattice structure anisotropy is big, makes pure lead titanate ceramics material in annealing process by being easy when curie point Generate micro-crack, it is difficult to which densified sintering product, the present invention is doped modification to it to solve the above-mentioned problems, and it is rare earth modified to mix samarium The Curie temperature of lead titanate piezoelectric ceramics is higher, and mechanical-electric coupling anisotropy is big.
(2) preparation of samarium doping lead titanates nano particle: samarium doping lead titanates is nanocrystalline with zirconia balls and ethyl alcohol It is then that it is dry at 70-80 DEG C with ball mill ball milling to form samarium doping lead titanates nano particle in polyethylene bottle, it obtains To samarium doping lead titanates nano particle.
Ball-milling method is a kind of mechanical stripping technology, environmentally protective, easy to operate, low cost.It avoids due to redox Method uses reducing agents potential hazards caused by experiment operator and environment such as strong acid and hydrazine hydrate.
(3) preparation of amido modified samarium doping lead titanates nano particle: by samarium doping lead titanates nano particle and poly- second Base maleimide powder distinguishes ultrasonic disperse in deionized water, and pH is adjusted to 9-11 respectively, obtains poly- ethyl Malaysia Imide solution and samarium doping metatitanic acid lead solution;Then poly- ethyl maleimide solution is added dropwise to the samarium doping titanium of dispersion In lead plumbate solution, 1-3h is stirred, amido modified samarium doping lead titanates nano particle is obtained after centrifuge separation, is washed with deionized water Excessive poly- ethyl maleimide is removed, then is washed with dehydrated alcohol to remove distilled water, centrifugation obtains pure amido modified Samarium doping lead titanates nano particle.
Samarium doping lead titanates piezoelectric nano-particles carry out surface functionalization with amino, it is ensured that with the Malaysia in polymer substrate Anhydride molecule covalent coupling.It, can be multiple in polymer containing amido modified nano particle compared with unmodified nanoparticles Being uniformly distributed in condensation material, and therefore improve piezo-electric generating.Flexible device based on this unique composite material manufacture exists The voltage generated during Cyclic flexion and not bending motion significantly improves.
(4) preparation of fiber base flexible piezoelectric sensors: being prepared by wet spinning, by amido modified samarium doping metatitanic acid Lead nano particle is dispersed in tetrahydrofuran solution and ultrasonic disperse 4-6h;S-B-S block copolymerization is added Object stirs 24-36 hours at 25-35 DEG C, then feeds the mixture into and reacts 9-10h into ptfe autoclave, reaction After the completion, it cools down, is finally ultrasonically treated in a water bath before fibre spinning 1-2 hours at room temperature, obtain spinning solution, select In the alcohol solidification bath that 10-20mL syringe with empty needle in No. 23 rotates spinning solution injection 5-10Hz, by gained fibre Dimension is vertically pulled out and is wrapped on spool, obtains fiber base flexible piezoelectric sensors.
Wet spinning is one of main spinning process of chemical fibre.Fiber-forming polymer is dissolved in solvent appropriate, is obtained To definite composition, certain viscosity and the solution with good spinnability, claim spinning solution.It can also directly be obtained by homogeneous solution polymerization To spinning solution.Spinning solution is sent by circulating line to spinning machine, by measuring pump-metered, then through candle filter, connecting tube And enter spinning head (cap).The stoste thread extruded from spinneret eyelet enters coagulating bath, and the solvent in stoste thread is to solidification Bath diffusion, coagulator permeate to thread, so that stoste thread be made to reach critical concentration, are precipitated in coagulating bath and form fiber.
Preferably, in step (1), in the mixed solution after the constant volume, [OH]=1.0-2.0molL-1, [3/2Sm +Pb]=0.15-0.20mol·L-l, [Ti]=0.1-0.2molL-1
Preferably, being warming up to 220-300 DEG C in step (1).
Preferably, taking out product in step (1) and being impregnated in deionized water and dehydrated alcohol, and wash repeatedly respectively 3-4 times.
Preferably, ball mill rotational speed of ball-mill is 15-45Hz in step (2), Ball-milling Time is 60-100 minutes.
Preferably, in step (3), the mass ratio of the poly- ethyl maleimide solution and samarium doping metatitanic acid lead solution For 1:10.
Preferably, in step (3), centrifugal rotational speed 8000-10000rpm.
Preferably, deionized water is washed 1-2 times in step (3), dehydrated alcohol is washed 3-4 times.
Preferably, the dosage of the tetrahydrofuran is 20-40mL in step (4).
Preferably, in step (4), the tetrahydrofuran 20-40mL, content 99%, ultrasonic processor S-450D- 1/2 processor, No. 23 hollow needle injections are used as spinning head.
It is compared with the prior art, the beneficial effects of the present invention are:
1, the present invention is nanocrystalline with samarium doping lead titanates, modified tradition lead titanate piezoelectric ceramics, with the metatitanic acid being widely used at present Lead piezoelectric ceramics are compared, and the Curie temperature for mixing the rare earth modified lead titanate piezoelectric ceramics of samarium is higher, and mechanical-electric coupling anisotropy is big, More suitable for the various energy converters to work under production high temperature, and use ball mill ball milling at nano particle, enlarged contact areas it.
2, samarium doping lead titanates piezoelectric nano-particles carry out surface functionalization with amino, it is ensured that with the horse in polymer substrate Carry out anhydride molecule covalent coupling.It, can be in polymer containing amido modified nano particle compared with unmodified nanoparticles Being uniformly distributed in composite material, and therefore improve piezo-electric generating.
3, flexible sensor of the present invention is spun into fiber based sensor using wet spinning, improves flexible and stability, And its stitchability expands the scope of application of sensor.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1
(1) the nanocrystalline preparation of samarium doping lead titanates:
Butyl titanate is added in ptfe autoclave, deionized water is added under agitation, obtains suspension Afterwards, sequentially add the aqueous solution of lead acetate, samarium trichloride, sodium hydroxide under agitation, all reactions with water be all made of from Sub- water, last constant volume is to 250ml, wherein [OH]=1.0molL-1, [3/2Sm+Pb]=0.15molL-l, [Ti]= 0.1mol·L-1,.Reaction kettle is heated and is stirred 4 minutes, is stirred for after heating 4 minutes, 220 DEG C at a temperature of keep the temperature 8h. To after the reaction was completed, reaction kettle be made to naturally cool to room temperature.It takes out in product and impregnates certain time, fill soluble ion Divide exchange, filtering and washing product washs 3 times repeatedly respectively in deionized water and dehydrated alcohol, removes soluble ion, then exist Dry 6h, it is nanocrystalline to obtain samarium doping lead titanates in 80 DEG C of baking oven.
(2) preparation of samarium doping lead titanates nano particle:
Samarium doping lead titanates it is nanocrystalline with zirconia balls and ethyl alcohol in polyethylene bottle with ball mill ball milling to form samarium doping Lead titanates nano particle, ball mill rotational speed of ball-mill are 15Hz, and Ball-milling Time is 60 minutes, then that it is dry at 70 DEG C.
(3) preparation of amido modified samarium doping lead titanates nano particle:
By samarium doping lead titanates nano particle that step (2) obtains and poly- ethyl maleimide powder, ultrasonic disperse is being gone respectively In ionized water, and the pH of solution is adjusted to 10 respectively, then poly- ethyl maleimide solution is added dropwise to the samarium of dispersion In doped titanic acid lead solution, the samarium doping metatitanic acid lead solution of the poly- ethyl maleimide solution dispersed in mixed solution and dispersion Mass ratio be 1:10, and mixed solution is stirred into 1h, after stirring, the centrifuge separation for being 8000 turns by revolving speed is prepared Amido modified samarium doping lead titanates nano particle, and be washed with deionized 1 time and wash away excessive poly- ethyl maleimide Amine, then after washing 3 times with dehydrated alcohol to remove distilled water, pass through the centrifuge centrifugation that revolving speed is 8000 turns and obtain pure ammonia The samarium doping lead titanates nano particle of base modification.
(4) preparation of fiber base flexible piezoelectric sensors:
It is prepared, nano particle prepared by step (3) is dispersed in tetrahydrofuran and with ultrasonic disperse 4h by wet spinning, four Hydrogen furans 20mL, content 99%.Then, it stirs 24 hours at 25 DEG C in gained suspension, finally makes before fibre spinning It is ultrasonically treated 1 hour with the output power of 45W in a water bath with digital ultrasound processor S-450D-1/2.Using in No. 23 The 10mL syringe of empty needle uses in the alcohol solidification bath for rotating spinning solution injection 5Hz as spinning head, by gained fiber It vertically pulls out and is wrapped on spool, obtain fiber base flexible piezoelectric sensors.
Embodiment 2
(1) the nanocrystalline preparation of samarium doping lead titanates:
Butyl titanate is added in ptfe autoclave, deionized water is added under agitation, obtains suspension Afterwards, sequentially add the aqueous solution of lead acetate, samarium trichloride, sodium hydroxide under agitation, all reactions with water be all made of from Sub- water, last constant volume is to 300ml, wherein [OH]=2.0molL-1, [3/2Sm+Pb]=0.20molL-l, [Ti]= 0.2mol·L-1,.Reaction kettle is heated and is stirred 5 minutes, is stirred for after heating 4 minutes, 220 DEG C at a temperature of keep the temperature 10h. To after the reaction was completed, reaction kettle be made to naturally cool to room temperature.It takes out in product and impregnates certain time, fill soluble ion Divide exchange, filtering and washing product washs 4 times repeatedly respectively in deionized water and dehydrated alcohol, removes soluble ion, then exist Dry 6h, it is nanocrystalline to obtain samarium doping lead titanates in 80 DEG C of baking oven.
(2) preparation of samarium doping lead titanates nano particle:
Samarium doping lead titanates it is nanocrystalline with zirconia balls and ethyl alcohol in polyethylene bottle with ball mill ball milling to form samarium doping Lead titanates nano particle, ball mill rotational speed of ball-mill are 15Hz, and Ball-milling Time is 100 minutes, then that it is dry at 80 DEG C.
(3) preparation of amido modified samarium doping lead titanates nano particle:
By samarium doping lead titanates nano particle that step (2) obtains and poly- ethyl maleimide powder, ultrasonic disperse is being gone respectively In ionized water, and the pH of solution is adjusted to 10 respectively, then poly- ethyl maleimide solution is added dropwise to the samarium of dispersion In doped titanic acid lead solution, the samarium doping metatitanic acid lead solution of the poly- ethyl maleimide solution dispersed in mixed solution and dispersion Mass ratio be 1:10, and mixed solution is stirred into 3h, after stirring, preparation is separated by the centrifuge that revolving speed is 10000 turns Good amido modified samarium doping lead titanates nano particle, and be washed with deionized 2 times and wash away excessive poly- ethyl Malaysia acyl Imines, then after washing 4 times with dehydrated alcohol to remove distilled water, the centrifuge centrifugation for being 10000 turns by revolving speed obtains pure Amido modified samarium doping lead titanates nano particle.
(4) preparation of fiber base flexible piezoelectric sensors:
It is prepared, nano particle prepared by step (3) is dispersed in tetrahydrofuran and with ultrasonic disperse 6h by wet spinning, four Hydrogen furans 40mL, content 99%.Then, it stirs 36 hours at 35 DEG C in gained suspension, finally makes before fibre spinning It is ultrasonically treated 2 hours with the output power of 67W in a water bath with digital ultrasound processor S-450D-1/2.Using in No. 23 The 20mL syringe of empty needle uses in the alcohol solidification bath for rotating spinning solution injection 10Hz as spinning head, by gained fiber It vertically pulls out and is wrapped on spool, obtain fiber base flexible piezoelectric sensors.
Embodiment 3
(1) the nanocrystalline preparation of samarium doping lead titanates:
Butyl titanate is added in ptfe autoclave, deionized water is added under stirring conditions, is suspended After liquid, the aqueous solution of lead acetate, samarium trichloride, sodium hydroxide is sequentially added under stirring conditions, and all reactions are all made of with water Deionized water, last constant volume is to 250ml, wherein [OH]=2.0molL-1, [3/2Sm+Pb]=0.15molL-l, [Ti]= 0.1mol·L-1,.Reaction kettle is heated and is stirred 4-5 minutes, is stirred for after heating 4 minutes, 300 DEG C at a temperature of keep the temperature 8h.To after the reaction was completed, reaction kettle be made to naturally cool to room temperature.It takes out in product and impregnates certain time, send out soluble ion Raw sufficiently exchange, filtering and washing product wash 3 times repeatedly respectively in deionized water and dehydrated alcohol, remove soluble ion, so The dry 8h in 100 DEG C of baking oven afterwards, it is nanocrystalline to obtain samarium doping lead titanates.
(2) preparation of samarium doping lead titanates nano particle:
Samarium doping lead titanates it is nanocrystalline with zirconia balls and ethyl alcohol in polyethylene bottle with ball mill ball milling to form samarium doping Lead titanates nano particle, ball mill rotational speed of ball-mill are 15Hz, and Ball-milling Time is 100 minutes, then that it is dry at 70 DEG C.
(3) preparation of amido modified samarium doping lead titanates nano particle:
By samarium doping lead titanates nano particle that step (2) obtains and poly- ethyl maleimide powder, ultrasonic disperse is being gone respectively In ionized water, and the pH of solution is adjusted to 10 respectively, then poly- ethyl maleimide solution is added dropwise to the samarium of dispersion In doped titanic acid lead solution, the samarium doping metatitanic acid lead solution of the poly- ethyl maleimide solution dispersed in mixed solution and dispersion Mass ratio be 1:10, and mixed solution is stirred into 3h, after stirring, preparation is separated by the centrifuge that revolving speed is 10000 turns Good amido modified samarium doping lead titanates nano particle, and be washed with deionized 1 time and wash away excessive poly- ethyl Malaysia acyl Imines, then after washing 3 times with dehydrated alcohol to remove distilled water, the centrifuge centrifugation for being 10000 turns by revolving speed obtains pure Amido modified samarium doping lead titanates nano particle.
(4) preparation of fiber base flexible piezoelectric sensors:
It is prepared, nano particle prepared by step (3) is dispersed in tetrahydrofuran and with ultrasonic disperse 4h by wet spinning, four Hydrogen furans 40mL, content 99%.Then, it stirs 24 hours at 25 DEG C in gained suspension, finally makes before fibre spinning It is ultrasonically treated 2 hours with the output power of 45-67W in a water bath with digital ultrasound processor S-450D-1/2.Using with 23 The 10mL syringe of empty needle uses in the alcohol solidification bath for rotating spinning solution injection 10Hz as spinning head in number, by gained Fiber is vertically pulled out and is wrapped on spool, obtains fiber base flexible piezoelectric sensors.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field;In the present invention Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side The protection scope of case.

Claims (9)

1. a kind of preparation method of fiber base flexible piezoelectric sensors, it is characterised in that include the following steps:
(1) the nanocrystalline preparation of samarium doping lead titanates: deionized water is added in butyl titanate under agitation, is suspended After liquid, the aqueous solution of lead acetate, samarium trichloride, sodium hydroxide is sequentially added under agitation, last constant volume to 250-300ml, Obtain mixed solution;Mixed solution is added to oil bath heating in reaction kettle and is stirred 4-5 minutes, 8-10h is kept the temperature after heating;To After the reaction was completed, room temperature is naturally cooled to, product is taken out and impregnates, makes soluble ion that sufficiently exchange occur, filtering and washing removes Soluble ion, the then dry 6-8h at 80-100 DEG C, being cooled to room temperature, to obtain samarium doping lead titanates nanocrystalline;
(2) preparation of samarium doping lead titanates nano particle: samarium doping lead titanates is nanocrystalline with zirconia balls and ethyl alcohol is poly- It is then that it is dry at 70-80 DEG C with ball mill ball milling to form samarium doping lead titanates nano particle in ethylene bottle, obtain samarium Doped with Titanium lead plumbate nano particle;
(3) preparation of amido modified samarium doping lead titanates nano particle: by samarium doping lead titanates nano particle and poly- ethyl horse Carry out acid imide powder difference ultrasonic disperse in deionized water, and pH is adjusted to 9-11 respectively, obtains poly- ethyl maleimide Amine aqueous solution and samarium doping metatitanic acid lead solution;Then poly- ethyl maleimide solution is added dropwise to the samarium doping lead titanates of dispersion In solution, 1-3h is stirred, amido modified samarium doping lead titanates nano particle is obtained after centrifuge separation, was washed with deionized water The poly- ethyl maleimide of amount, then washed with dehydrated alcohol to remove distilled water, centrifugation obtains pure amido modified samarium Doped with Titanium lead plumbate nano particle;
(4) amido modified samarium doping lead titanates nano particle the preparation of fiber base flexible piezoelectric sensors: is dispersed in tetrahydro In tetrahydrofuran solution and ultrasonic disperse 4-6h;Styrene-Butadiene-Styrene Block Copolymer is added and stirs 24- at 25-35 DEG C It 36 hours, then feeds the mixture into and reacts 9-10h into ptfe autoclave, after the reaction was completed, cool down at room temperature, It is finally ultrasonically treated in a water bath before fibre spinning 1-2 hours, obtains spinning solution, select the 10- with empty needle in No. 23 Gained fiber is vertically pulled out in the alcohol solidification bath of spinning solution injection 5-10Hz rotation and is wound online by 20mL syringe On axis, fiber base flexible piezoelectric sensors are obtained.
2. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (1) In, in the mixed solution after the constant volume, [OH]=1.0-2.0molL-1, [3/2Sm+Pb]=0.15-0.20molL-l, [Ti]=0.1-0.2mol·L-1
3. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (1) In, it is warming up to 220-300 DEG C.
4. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (1) In, it takes out product and is impregnated in deionized water and dehydrated alcohol, and wash 3-4 times repeatedly respectively.
5. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (2) In, ball mill rotational speed of ball-mill is 15-45Hz, and Ball-milling Time is 60-100 minutes.
6. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (3) In, the mass ratio of the poly- ethyl maleimide solution and samarium doping metatitanic acid lead solution is 1:10.
7. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (3) In, centrifugal rotational speed 8000-10000rpm.
8. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (3) In, deionized water is washed 1-2 times, and dehydrated alcohol washs 3-4 times.
9. a kind of preparation method of fiber base flexible piezoelectric sensors as described in claim 1, which is characterized in that step (4) In, the dosage of the tetrahydrofuran is 20-40mL.
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CN110923839A (en) * 2019-11-21 2020-03-27 台州市旭泓服饰有限公司 Elastic cotton textile fiber and preparation method thereof
CN111747740A (en) * 2020-06-28 2020-10-09 安徽容知日新科技股份有限公司 Samarium ion doped lead zirconate titanate based high-performance piezoelectric ceramic and preparation method thereof
CN114181565A (en) * 2021-10-21 2022-03-15 嘉兴聚鑫隆科技有限公司 Piezoelectric substrate for flexible sensor and manufacturing process thereof
CN117782379A (en) * 2024-02-27 2024-03-29 太原理工大学 Piezoelectric/pyroelectric dual-function flexible high-temperature-resistant sensor

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Application publication date: 20190108