CN104032374A - Preparation method of lead titanate/zinc oxide composite nanostructure on flexible substrate - Google Patents
Preparation method of lead titanate/zinc oxide composite nanostructure on flexible substrate Download PDFInfo
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Abstract
The invention discloses a preparation method of a lead titanate/zinc oxide composite nanostructure on a flexible substrate. The preparation method comprises the steps: preparing a powdery one-dimensional columnar-structure lead titanate monocrystal nanofiber by using a hydrothermal method, adding absolute ethyl alcohol, carrying out ultrasonic oscillation into a suspension, dripping onto a silicon slice, drying, annealing, to obtain a tetragonal-phase lead titanate monocrystal nanofiber, scraping down from the silicon slice, adding absolute ethyl alcohol, dripping onto the flexible substrate, and forming a lead titanate monocrystal nanofiber film on the flexible substrate; and then taking zinc acetate as a zinc oxide seed solution, taking a mixed solution of a zinc nitrate aqueous solution, a hexamethylentetramine aqueous solution and a sodium citrate aqueous solution as a zinc oxide growing solution, growing zinc oxide on the flexible substrate with the lead titanate monocrystal nanofiber film, and thus obtaining the lead titanate/zinc oxide composite nanostructure on the flexible substrate. The preparation method has the advantages of simple technological process, easy control, no pollution and low cost. The prepared lead titanate/zinc oxide composite nanostructure on the flexible substrate is high in purity and good in dispersion.
Description
Technical field
the present invention relates to a kind of preparation method of lead titanate/zinc oxide composite nanostructure, relate in particular to the preparation method of lead titanate/zinc oxide composite nanostructure in a kind of flexible substrates.
Background technology
Lead titanate is a kind of typical perovskite typed ferroelectric oxide, due to simple in structure, piezoelectricity and ferroelectricity are strong, since finding the fifties, lead titanate is ferroelectric and former shaped material piezoelectricity area research always, for people, is familiar with perovskite oxide piezoelectricity and ferroelectric electronics origin has very important meaning.In addition, it also has very large application potential as pyroelectricity material, is up-and-coming ferroelectric, piezoelectricity and pyroelectricity material.Zhejiang University is used polymer assisting alcohol-hydrothermal method to make lead titanate monocrystal nano fiber (Zhaohui Ren, Gang Xu, the Yong Liu of one-dimensional columnar structure first, Xiao Wei, Yihan Zhu, Xiaobin Zhang, Guanglie Lv, Youwen Wang, Yuewu Zeng, Piyi Du, Wenjian Weng, Ge Shen, J. Z. Jiang and Gaorong Han, PbTiO
3nanofibers with Edge-Shared TiO
6octahedra, 2010,132 (16), 5572-5573.).The lead titanate crystal of this structure, its titanyl octahedral body is to be connected to form one-dimensional columnar structure by common limit.This one-dimensional columnar structure lead titanate, after certain condition anneal, can be phase-changed into Tetragonal (P4mm) lead titanate, keeps the pattern of 1-dimention nano fiber simultaneously.But for the research of the matrix material of this material and other oxide compounds, the preparation and property that especially carries out matrix material on flexible base is probed at present still in the exploratory stage, is showed no relevant report both at home and abroad.
Summary of the invention
the object of the present invention is to provide that a kind of technique is simple, the preparation method of the lead titanate/zinc oxide composite nanostructure in the flexible substrates that is easy to control.
in flexible substrates of the present invention, the preparation method of lead titanate/zinc oxide composite nanostructure, comprises the steps:
1) by the chemical formula PbTiO of the synthetic one-dimensional columnar structure lead titanate monocrystal nano fiber of wish
3metering, takes lead nitrate and is dissolved in deionized water, regulates Pb
2+ionic concn is 0.25-1mol/L;
Butyl (tetra) titanate is dissolved in to ethylene glycol monomethyl ether, the Ti in regulator solution
4+ionic concn is 0.25-1mol/L, adds the ammoniacal liquor of mass concentration 30% to Ti
4+ion precipitates completely, filters, cleans, obtains the oxyhydroxide precipitation of titanium;
2) configure respectively the potassium hydroxide aqueous solution of 0.5-5mol/L and the polyvinyl alcohol water solution that concentration is 2g/L, by the oxyhydroxide precipitation of potassium hydroxide aqueous solution, polyvinyl alcohol water solution, titanium and step 1) the lead nitrate aqueous solution join together in reactor inner bag, the volume ratio of potassium hydroxide aqueous solution, polyvinyl alcohol water solution and the lead nitrate aqueous solution is 1:2:1, Ti
4+with Pb in lead nitrate solution
2+mol ratio is 1:1, and reactor inner bag is placed in to reactor, airtight, is placed in 180-200
oin the stove of C, after insulation reaction 8-12 hour, be placed in air and be naturally cooled to room temperature, take out reaction product, filter, by washed with de-ionized water, dry, obtain Powdered one-dimensional columnar structure lead titanate monocrystal nano fiber;
3) by step 2) to be added to volume be step 2 for the Powdered one-dimensional columnar structure lead titanate monocrystal nano fiber that makes) in the dehydrated alcohol of 0.25 ~ 1 times of lead nitrate aqueous solution volume, ultra-sonic oscillation obtain suspension, dropped on the silicon chip through cleaning and be paved with to it, dry, again by hanging drop to silicon chip, dry, repeat 4 ~ 5 times, subsequently silicon chip is incubated at least 1.5h in 600 ~ 750 ℃, cooling rear taking-up obtains Tetragonal lead titanate monocrystal nano fiber on silicon chip;
4) Tetragonal lead titanate monocrystal nano tunica fibrosa step 3) being obtained scrapes from silicon chip, being added to volume is step 2) in the dehydrated alcohol of 0.25 ~ 1 times of lead nitrate aqueous solution volume, ultra-sonic oscillation obtain suspension, dropped in the flexible substrates through cleaning and be paved with to it, dry, again by hanging drop to flexible substrates, dry, repeat 4 ~ 5 times, in flexible substrates, form lead titanate monocrystal nano tunica fibrosa;
5) zinc acetate aqueous solution of configuration 0.001 ~ 0.01mol/L, and drop in the flexible substrates with lead titanate monocrystal nano tunica fibrosa of step 4) and be paved with to it, dry, again zinc acetate aqueous solution is dropped in flexible substrates, dry, repeat 4 ~ 5 times, then it is incubated to 0.5 ~ 2h in 100 ℃;
6) configure respectively the zinc nitrate aqueous solution of 0.001mol/L ~ 0.1mol/L, the hexamethylenetetramine aqueous solution of 0.001mol/L-0.1mol/L and the sodium citrate aqueous solution of 2 ~ 80mM/L, and by zinc nitrate aqueous solution, the hexamethylenetetramine aqueous solution and sodium citrate aqueous solution by volume 20:20:1 be mixed to join in reaction vessel, the flexible substrates of processing through step 5) is immersed to mixed solution, sealing, in 85 ~ 100 ℃ of insulation 0.5 ~ 12h, cooling rear taking-up, clean and dry, obtain the lead titanate/zinc oxide composite nanostructure in flexible substrates.
In the present invention, described flexible substrates can be polyethylene terephthalate (PET), polycarbonate (PC), PEN (PEN) or polyimide (PI).
Described lead nitrate, butyl (tetra) titanate, potassium hydroxide, polyvinyl alcohol, zinc acetate, zinc nitrate, hexamethylenetetramine, dehydrated alcohol and Trisodium Citrate purity are all not less than chemical pure.
Described reactor is to have polytetrafluoroethylliner liner and adopt the reactor that stainless steel external member is airtight.
Technological process of the present invention is simple, is easy to control, and pollution-free, cost is low, and in the flexible substrates making, lead titanate/zinc oxide composite nanostructure purity is high, good dispersity.The preparation that can be the matrix material of perovskite oxide and conductor oxidate provides development foundation.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the upper lead titanate/zinc oxide composite nanostructure of the PET that makes of embodiment 1.
Fig. 2 is the scanning electron microscope picture of the upper lead titanate/zinc oxide composite nanostructure of the PET that makes of embodiment 1.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1) configuration Pb
2+ionic concn is the lead nitrate aqueous solution 20ml of 0.25mol/L; Butyl (tetra) titanate is dissolved in to ethylene glycol monomethyl ether, makes the Ti in solution
4+ionic concn is 0.25mol/L, adds the ammoniacal liquor of mass concentration 30% to Ti
4+ion precipitates completely, filters, cleans, obtains the oxyhydroxide precipitation of titanium;
2) configure respectively the potassium hydroxide aqueous solution 20ml of 1mol/L and the polyvinyl alcohol water solution 40ml of 2g/L, by the oxyhydroxide precipitation of potassium hydroxide aqueous solution, polyvinyl alcohol water solution, titanium and step 1) the lead nitrate aqueous solution join together in reactor inner bag, Ti
4+with Pb in lead nitrate solution
2+mol ratio is 1:1, is placed in reactor, airtight, in 180
oin the stove of C, be incubated, react after 12 hours, be placed in air and be naturally cooled to room temperature, take out reaction product, filter, by washed with de-ionized water, dry, obtain powdery one-dimensional columnar structure lead titanate monocrystal nano fiber;
3) by step 2) the powdery one-dimensional columnar structure lead titanate monocrystal nano fiber that makes joins in 5mL dehydrated alcohol, and ultra-sonic oscillation obtain scattered suspension, and hanging drop is added to 3 * 3cm through cleaning
2on silicon chip, to it, be paved with, be placed under infrared lamp dry, again by hanging drop to silicon chip, dry, so repeat, after 4 times, on silicon chip, to form lead titanate monocrystal nano tunica fibrosa, put into subsequently retort furnace 750
oc is incubated 1.5h, takes out after being cooled to room temperature, makes product become mutually Tetragonal lead titanate monocrystal nano fiber;
4) Tetragonal lead titanate monocrystal nano tunica fibrosa step 3) being obtained scrapes from silicon chip, be added in 5mL dehydrated alcohol, ultra-sonic oscillation obtain disperseing good suspension, the PET that hanging drop is added to through cleaning is above paved with to it, be placed under infrared lamp dry, again hanging drop is upper to PET, dry, so repeat 4 times, on PET, form lead titanate monocrystal nano tunica fibrosa;
5) zinc acetate aqueous solution that configuration concentration is 0.01mol/L is as secondary oxidative zinc seed solution, and the PET with lead titanate monocrystal nano tunica fibrosa that this seed solution is dropped to step 4) is above paved with to it, is placed in loft drier 60
oc is dried 5min, again zinc acetate aqueous solution is dropped to PET upper, dry, so repeats 4 times, and the sample of handling well is placed in to retort furnace in 100
oc is incubated 30min, takes out after being cooled to room temperature;
6) configure respectively the hexamethylenetetramine aqueous solution 40ml of zinc nitrate aqueous solution 40ml, 0.05mol/L and the sodium citrate aqueous solution 2ml of 20mM/L of 0.05mol/L, and they are mixed and are placed in reaction vessel as zinc oxide growth liquid, sample that step 5) is handled well immerses and fills in the container of growth media, and preservative film sealing is placed in insulation can 90
oc, is cooled to room temperature after insulation 2h naturally, takes out sample, by washed with de-ionized water, dries, and obtains lead titanate/zinc oxide composite nanostructure on PET.
The XRD spectral line of the upper lead titanate/zinc oxide composite nanostructure of PET that this example makes as shown in Figure 1, can find out that sample crystallization degree is good, the diffraction peak simultaneously with Tetragonal (P4mm) lead titanate and wurtzite zinc oxide, shows that product is the compound of bi-material.As shown in Figure 2, lead titanate/zinc oxide composite nanostructure is uniformly distributed corresponding SEM photo on PET.Upper lead titanate/the zinc oxide composite nanostructure of PET making can bear compared with large deformation, has good snappiness.
Embodiment 2
1) configuration Pb
2+ionic concn is the lead nitrate aqueous solution 20ml of 0.5mol/L; Butyl (tetra) titanate is dissolved in to ethylene glycol monomethyl ether, makes the Ti in solution
4+concentration is 0. 5mol/L, adds the ammoniacal liquor of mass concentration 30% to Ti
4+ion precipitates completely, filters and cleans the oxyhydroxide precipitation that obtains titanium;
2) configure respectively the potassium hydroxide aqueous solution 20ml of 0.5mol/L and the polyvinyl alcohol water solution 40ml of 2g/L, by the oxyhydroxide precipitation of potassium hydroxide aqueous solution, polyvinyl alcohol water solution, titanium and step 1) the lead nitrate aqueous solution join together in reactor inner bag, Ti
4+with Pb in lead nitrate solution
2+mol ratio is 1:1, is placed in reactor, airtight, in 200
oin the stove of C, be incubated, react after 12 hours, be placed in air and be naturally cooled to room temperature, take out reaction product, filter, by washed with de-ionized water, dry, obtain powdery one-dimensional columnar structure lead titanate monocrystal nano fiber;
3) in step 2) add 10mL dehydrated alcohol in the powdery one-dimensional columnar structure lead titanate monocrystal nano fiber that makes, ultra-sonic oscillation obtain scattered suspension, drop to 3 * 3cm through cleaning
2on silicon chip, to it, be paved with, be placed under infrared lamp dry 5min, again by hanging drop to silicon chip, dry, repeat, after 4 times, on silicon chip, to form lead titanate monocrystal nano tunica fibrosa, put into subsequently retort furnace 650
oc is incubated 2h, takes out after being cooled to room temperature, makes product become mutually Tetragonal lead titanate monocrystal nano fiber.
4) Tetragonal lead titanate monocrystal nano tunica fibrosa step 3) being obtained scrapes from silicon chip, add 5mL dehydrated alcohol, ultra-sonic oscillation obtain disperseing good suspension, the PC that hanging drop is added to through cleaning is above paved with to it, be placed under infrared lamp dry, again hanging drop is upper to PC, dry, so repeat 4 times, on PC, form lead titanate monocrystal nano tunica fibrosa;
5) zinc acetate aqueous solution that configuration concentration is 0.005mol/L is as secondary oxidative zinc seed solution, and the PC with lead titanate monocrystal nano tunica fibrosa that this seed solution is dropped to step 4) is above paved with to it, is placed in loft drier 60
oc is dried 5min, again zinc acetate aqueous solution is dropped to PC upper, dry, so repeats 4 times, and the sample of handling well is placed in to retort furnace in 100
oc is incubated 2h, takes out after being cooled to room temperature;
6) configure respectively the hexamethylenetetramine aqueous solution 20ml of zinc nitrate aqueous solution 20ml, 0.001mol/L and the sodium citrate aqueous solution 1ml of 2mM/L of 0.001mol/L, and they are mixed and are placed in reaction vessel as zinc oxide growth liquid, sample that step 5) is handled well immerses and fills in the container of growth media, and preservative film sealing is placed in insulation can 85
oc, is cooled to room temperature after insulation 12h naturally, takes out sample, by washed with de-ionized water, dries, and obtains lead titanate/zinc oxide composite nanostructure on PC.
Embodiment 3
1) configuration Pb
2+ionic concn is the lead nitrate aqueous solution 20ml of 1mol/L; Butyl (tetra) titanate is dissolved in to ethylene glycol monomethyl ether, makes Ti in solution
4+concentration is 1mol/L, adds the ammoniacal liquor of mass concentration 30% to Ti
4+ion precipitates completely, filters and cleans the oxyhydroxide precipitation that obtains titanium;
2) configure respectively the potassium hydroxide aqueous solution 20ml of 2mol/L and the polyvinyl alcohol water solution 40ml of 2g/L, by the oxyhydroxide precipitation of potassium hydroxide aqueous solution, polyvinyl alcohol water solution, titanium and step 1) the lead nitrate aqueous solution join together in reactor inner bag, Ti
4+with Pb in lead nitrate solution
2+mol ratio is 1:1, is placed in reactor, airtight, in 200
oin the stove of C, be incubated, react after 10 hours, be placed in air and be naturally cooled to room temperature, take out reaction product, filter, by washed with de-ionized water, dry, obtain powdery one-dimensional columnar structure lead titanate monocrystal nano fiber;
3) in step 2) add 20mL dehydrated alcohol in the powdery one-dimensional columnar structure lead titanate monocrystal nano fiber that makes, ultra-sonic oscillation obtain suspension, and hanging drop is added to 3 * 3cm through cleaning
2on silicon chip, to it, be paved with, be placed in 60
odry 5min under C infrared lamp, again by hanging drop to silicon chip, dry, so repeat 5 times, on silicon chip, form lead titanate monocrystal nano tunica fibrosa, put into subsequently retort furnace 600
oc is incubated 4h, takes out after being cooled to room temperature, makes product become mutually Tetragonal lead titanate monocrystal nano fiber;
4) Tetragonal lead titanate monocrystal nano tunica fibrosa step 3) being obtained scrapes from silicon chip, add 10mL dehydrated alcohol, ultra-sonic oscillation obtain suspension, the PEN that hanging drop is added to through cleaning is above paved with to it, be placed under infrared lamp dry, again hanging drop is upper to PEN, dry, so repeat 5 times, on PEN, form lead titanate monocrystal nano tunica fibrosa;
5) zinc acetate aqueous solution that configuration concentration is 0.001mol/L is as secondary oxidative zinc seed solution, and the PEN with lead titanate monocrystal nano tunica fibrosa that this seed solution is dropped to step 4) is above paved with to it, is placed in loft drier 60
oc is dried 5min, again zinc acetate aqueous solution is dropped to PEN upper, dry, so repeats 5 times, and the sample of handling well is placed in to retort furnace 100
oc is incubated 1h, takes out after being cooled to room temperature;
6) configure respectively the hexamethylenetetramine aqueous solution 40ml of zinc nitrate aqueous solution 40ml, the 0.05mol/L of 0.05mol/L, and the sodium citrate aqueous solution 2ml of 20mM/L, and they are mixed and are placed in reaction vessel as zinc oxide growth liquid, sample that step 5) is handled well immerses and fills in the container of growth media, and preservative film sealing is placed in insulation can 90
oc, is cooled to room temperature after insulation 4h naturally, takes out sample, by washed with de-ionized water, dries, and obtains lead titanate/zinc oxide composite nanostructure on PEN.
Embodiment 4
1) configuration Pb
2+ionic concn is the lead nitrate aqueous solution 20ml of 0.75mol/L; Butyl (tetra) titanate is dissolved in to ethylene glycol monomethyl ether, makes Ti in solution
4+concentration is 0.75mol/L, adds the ammoniacal liquor of mass concentration 30% to Ti
4+ion precipitates completely, filters and cleans the oxyhydroxide precipitation that obtains titanium;
2) the polyvinyl alcohol water solution 40ml of potassium hydroxide aqueous solution 20ml, 2g/L that configures respectively 5mol/L is by the oxyhydroxide precipitation of potassium hydroxide aqueous solution, polyvinyl alcohol water solution, titanium and step 1) the lead nitrate aqueous solution join together in reactor inner bag, Ti
4+with Pb in lead nitrate solution
2+mol ratio is 1:1, is placed in reactor, airtight, in 200
oin the stove of C, be incubated, react after 8 hours, be placed in air and be naturally cooled to room temperature, take out reaction product, filter, by washed with de-ionized water, dry, obtain powdery one-dimensional columnar structure lead titanate monocrystal nano fiber;
3) in step 2) add 10mL dehydrated alcohol in the powdery one-dimensional columnar structure lead titanate monocrystal nano fiber that makes, ultra-sonic oscillation obtain scattered suspension, and hanging drop is added to 3 * 3cm through cleaning
2on silicon chip, to it, be paved with, be placed under infrared lamp dry 5min, again by hanging drop to silicon chip, dry, so repeat, after 5 times, on silicon chip, to form lead titanate monocrystal nano tunica fibrosa, put into subsequently retort furnace in 700
oc is incubated 2h, takes out after being cooled to room temperature, makes product become mutually Tetragonal lead titanate monocrystal nano fiber;
4) the Tetragonal lead titanate monocrystal nano tunica fibrosa obtaining in step 3) is scraped from silicon chip, add 20mL dehydrated alcohol, ultra-sonic oscillation obtain disperseing good suspension, the PI that hanging drop is added to through cleaning is above paved with to it, be placed under infrared lamp dry, again hanging drop is upper to PI, dry, so repeat 4 times, on PI, form lead titanate monocrystal nano tunica fibrosa;
5) zinc acetate aqueous solution that configuration concentration is 0.005mol/L is as secondary oxidative zinc seed solution, and the PI that has lead titanate monocrystal nano tunica fibrosa that this seed solution is dropped to step 4) is above paved with to it, is placed in loft drier 60
oc is dried 5min, again zinc acetate aqueous solution is dropped to PI upper, dry, so repeats 4 times, and the sample of handling well is placed in to retort furnace in 100
oc is incubated 30min, takes out after being cooled to room temperature;
6) configure respectively the hexamethylenetetramine aqueous solution 40ml of zinc nitrate aqueous solution 40ml, the 0.1mol/L of 0.1mol/L, and the sodium citrate aqueous solution 2ml of 80mM/L, and they are mixed and are placed in reaction vessel as zinc oxide growth liquid, sample that step 5) is handled well immerses and fills in the container of growth media, and preservative film sealing is placed in insulation can 100
oc, is cooled to room temperature after insulation 0.5h naturally, takes out sample, by washed with de-ionized water, dries, and obtains lead titanate/zinc oxide composite nanostructure on PI.
Claims (4)
1. a preparation method for lead titanate/zinc oxide composite nanostructure in flexible substrates, is characterized in that comprising the steps:
1) by the chemical formula PbTiO of the synthetic one-dimensional columnar structure lead titanate monocrystal nano fiber of wish
3metering, takes lead nitrate and is dissolved in deionized water, regulates Pb
2+ionic concn is 0.25-1mol/L;
Butyl (tetra) titanate is dissolved in to ethylene glycol monomethyl ether, the Ti in regulator solution
4+ionic concn is 0.25-1mol/L, adds the ammoniacal liquor of mass concentration 30% to Ti
4+ion precipitates completely, filters, cleans, obtains the oxyhydroxide precipitation of titanium;
2) configure respectively the potassium hydroxide aqueous solution of 0.5-5mol/L and the polyvinyl alcohol water solution that concentration is 2g/L, by the oxyhydroxide precipitation of potassium hydroxide aqueous solution, polyvinyl alcohol water solution, titanium and step 1) the lead nitrate aqueous solution join together in reactor inner bag, the volume ratio of potassium hydroxide aqueous solution, polyvinyl alcohol water solution and the lead nitrate aqueous solution is 1:2:1, Ti
4+with Pb in lead nitrate solution
2+mol ratio is 1:1, and reactor inner bag is placed in to reactor, airtight, is placed in 180-200
oin the stove of C, after insulation reaction 8-12 hour, be placed in air and be naturally cooled to room temperature, take out reaction product, filter, by washed with de-ionized water, dry, obtain Powdered one-dimensional columnar structure lead titanate monocrystal nano fiber;
3) by step 2) to be added to volume be step 2 for the Powdered one-dimensional columnar structure lead titanate monocrystal nano fiber that makes) in the dehydrated alcohol of 0.25 ~ 1 times of lead nitrate aqueous solution volume, ultra-sonic oscillation obtain suspension, dropped on the silicon chip through cleaning and be paved with to it, dry, again by hanging drop to silicon chip, dry, repeat 4 ~ 5 times, subsequently silicon chip is incubated at least 1.5h in 600 ~ 750 ℃, cooling rear taking-up obtains Tetragonal lead titanate monocrystal nano fiber on silicon chip;
4) Tetragonal lead titanate monocrystal nano tunica fibrosa step 3) being obtained scrapes from silicon chip, being added to volume is step 2) in the dehydrated alcohol of 0.25 ~ 1 times of lead nitrate aqueous solution volume, ultra-sonic oscillation obtain suspension, dropped in the flexible substrates through cleaning and be paved with to it, dry, again by hanging drop to flexible substrates, dry, repeat 4 ~ 5 times, in flexible substrates, form lead titanate monocrystal nano tunica fibrosa;
5) zinc acetate aqueous solution of configuration 0.001 ~ 0.01mol/L, and drop in the flexible substrates with lead titanate monocrystal nano tunica fibrosa of step 4) and be paved with to it, dry, again zinc acetate aqueous solution is dropped in flexible substrates, dry, repeat 4 ~ 5 times, then it is incubated to 0.5 ~ 2h in 100 ℃;
6) configure respectively the zinc nitrate aqueous solution of 0.001mol/L ~ 0.1mol/L, the hexamethylenetetramine aqueous solution of 0.001mol/L-0.1mol/L and the sodium citrate aqueous solution of 2 ~ 80mM/L, and by zinc nitrate aqueous solution, the hexamethylenetetramine aqueous solution and sodium citrate aqueous solution by volume 20:20:1 be mixed to join in reaction vessel, the flexible substrates of processing through step 5) is immersed to mixed solution, sealing, in 85 ~ 100 ℃ of insulation 0.5 ~ 12h, cooling rear taking-up, clean and dry, obtain the lead titanate/zinc oxide composite nanostructure in flexible substrates.
2. according to the preparation method of lead titanate/zinc oxide composite nanostructure in the flexible substrates described in claims 1, it is characterized in that described flexible substrates is polyethylene terephthalate, polycarbonate, PEN or polyimide.
3. according to the preparation method of lead titanate/zinc oxide composite nanostructure in the flexible substrates described in claims 1, it is characterized in that the purity of described lead nitrate, butyl (tetra) titanate, potassium hydroxide, polyvinyl alcohol, zinc acetate, zinc nitrate, hexamethylenetetramine, dehydrated alcohol and Trisodium Citrate is all not less than chemical pure.
4. according to the preparation method of lead titanate/zinc oxide composite nanostructure in the flexible substrates described in claims 1, it is characterized in that described reactor is to have polytetrafluoroethylliner liner and adopt the reactor that stainless steel external member is airtight.
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| CN112816581A (en) * | 2020-12-30 | 2021-05-18 | 浙江大学 | Method for detecting halogenated quinoneimine in drinking water by derivatization-solid phase extraction-liquid chromatography tandem mass spectrometry |
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| 曹茂盛等: "高性能PZT压电厚膜及MEMS微驱动器技术研究", 《黑龙江大学工程学报》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112444542A (en) * | 2019-08-28 | 2021-03-05 | 河海大学 | Bismuth oxybromide/zinc oxide ITO electrode and application and preparation method thereof |
| CN112444542B (en) * | 2019-08-28 | 2022-02-11 | 河海大学 | Bismuth oxybromide/zinc oxide ITO electrode and application and preparation method thereof |
| CN112816581A (en) * | 2020-12-30 | 2021-05-18 | 浙江大学 | Method for detecting halogenated quinoneimine in drinking water by derivatization-solid phase extraction-liquid chromatography tandem mass spectrometry |
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| CN104032374B (en) | 2016-09-28 |
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