CN102704039A - Preparation method of polyethylene glycol/ZnO/Ag nanoparticle composite fiber material - Google Patents
Preparation method of polyethylene glycol/ZnO/Ag nanoparticle composite fiber material Download PDFInfo
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- CN102704039A CN102704039A CN2012101792070A CN201210179207A CN102704039A CN 102704039 A CN102704039 A CN 102704039A CN 2012101792070 A CN2012101792070 A CN 2012101792070A CN 201210179207 A CN201210179207 A CN 201210179207A CN 102704039 A CN102704039 A CN 102704039A
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Abstract
The invention relates to the technical field of preparation of nanomaterials, in particular to a preparation method of a polyethylene glycol/ZnO/Ag nanoparticle composite fiber, and aims to provide the preparation method of a polyethylene glycol/ZnO/Ag nanoparticle composite fiber material. The preparation method comprises the following steps of: preparing spinning solution; preparing [PEG+PVP]/[Zn(NO3)2+AgNO3] composite nanofiber; and preparing ZnO/Ag composite nanofiber. The method has the advantages of simple process, low cost and capabilities of improving the dispersibility of the nanoparticles in polymer solution and the uniformity of the obtained fiber and being applied to a gas sensitive sensor.
Description
Technical field
The present invention relates to the nano material preparation technical field, the preparation method of particularly a kind of polyethylene glycol/ZnO/Ag nano particle composite fibre is applied to the gas sensor field.
Background technology
In recent years, along with the development of photoelectric technology, device miniaturization and film change into and are a kind of trend, nano material and nano particle composite material optoelectronic areas application receive the extensive attention of scientific circles; The polymer nanofiber that preparation contains inorganic nano-particle receives much concern especially; Because this nano-complex combined the special performance (like the height ratio of surface atom and inner atom and quantum size effect etc.) of inorganic nano-particle and the excellent properties of polymer nanofiber (as very high specific area and in other materials height penetrability etc.); Like polyvinyl alcohol (PVA)/ZnO; PEO/ZnO, PVA/CdTe, PVA/CdSe etc.
ZnO is a kind of semiconductor material with wide forbidden band of direct band gap, and it is widely used in numerous areas such as electronics, sensor, dielectric material, ultraviolet shielded material, vacuum fluorescent display; The Ag nano particle is because its special electronic structure and huge specific area make it at the catalysis of chemical reaction, SERS, sensing, biomarker, aspect such as antibiotic important use arranged.
Electrostatic spinning technique is that the high polymeric solution of non-newtonian fluid overcomes surface tension and viscoplasticity power under high voltage electric field, carries out the stretch bending campaign and obtains the technology of nanometer to Sub-micro Fibers; This technology has that equipment is simple, and production cost is low, and materials used extensively reaches advantages such as specific area is big; At present, the existing both at home and abroad report that utilizes the coaxial electrostatic spinning silk device to prepare metal oxide, but the coaxial electrostatic spinning equipment is comparatively complicated, and all there is difficulty in the setting of choice of Solvent and spinning parameter, and single shaft static spins and has then overcome above deficiency.
The ZnO/Ag composite nano materials can be used as OPTICAL PROPERTIES, gas sensing modulator material, anti-microbial property research etc.; The ZnO/Ag composite nano materials of report all is film or nano particle at present, and the preparation method comprises: (1) ZnO nanocrystal surface reduction Ag
+Method (preparing the ZnO/Ag composite nanometer particle) [Xu Lihong etc., Physical Experiment, 2011,31 (10)]; (2) (with the polyvinylpyrrolidone is surfactant to one step hydro thermal method; Ethylene glycol solution with zinc acetate and silver nitrate slowly drops in the ethylene glycol successively, promptly obtains zinc oxide composite particles [Zhang Guoqing etc., material Leader that nano silver particles coats behind the high temperature reflux certain hour; 2010,24]; (3) solvent-thermal method (utilize ethanol, silver nitrate and zinc acetate to react and prepare ZnO surface deposition Ag nano particle) [Chen Shuan etc., chemistry world, 2011,52 (1)]; (4) high-molecular gel method (having prepared the ZnO/Ag composite nanometer particle) [Shao Zhongbao etc., investigation of materials journal, 2005,190 (01): 59-63]; (5) photo-reduction sedimentation (having prepared the ZnO/Ag composite nanometer particle) [well is upright strong etc., catalysis journal, 2002,23 (4): 336-340]; (6) chemical deposition (prepared the Ag particle deposition on the ZnO microsphere, and its air-sensitive performance is studied) [Guoxing Zhu etc., The Royal Society of Chemistry 2011].
Summary of the invention
Preparation ZnO/Ag composite nano materials in background technology; High-molecular gel method, chemical deposition, solvent-thermal method, one step hydro thermal method etc. have been adopted; The preparation method who the purpose of this invention is to provide a kind of polyethylene glycol/ZnO/Ag nano particle complex fiber material; This method technology is simple, cost is low, has improved the uniformity of nano particle dispersed and gained fiber in polymer solution, and has been applied to gas sensor.
The preparation method of a kind of polyethylene glycol of the present invention/ZnO/Ag nano particle complex fiber material comprises:
One, preparing spinning solution
What used in the zinc source in the spinning solution is zinc salt, is [Zn (NO
3)
26H
2O]; That use in the silver source is silver nitrate [AgNO
3]; High polymer templates adopts the mixture of polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP); Solvent adopts absolute ethyl alcohol and deionized water.
Take by weighing a certain amount of polyethylene glycol and polyvinylpyrrolidone and be dissolved in the absolute ethyl alcohol, mix again with through the zinc nitrate hexahydrate of ultrasonic dissolution and the mixed aqueous solution of silver nitrate, stir 4 ~ 10 h in the room temperature lower magnetic force, and leave standstill 2 ~ 6 h, promptly form spinning solution; The mass ratio of this each part of spinning solution is: [Zn (NO
3)
26H
2O+ AgNO
3]/[PEG+PVP]/absolute ethyl alcohol/deionized water=4:3:30:10, wherein the mass ratio of PEG and PVP is 2:1, AgNO
3With Zn (NO
3)
26H
2The amount of substance ratio of O is 0 ~ 0.1:1.
Two, preparation [PEG+PVP]/[Zn (NO
3)
2+ AgNO
3] composite nano fiber
Adopt electrostatic spinning technique, technical parameter is: DC voltage is: 15 ~ 20kV; The syringe needle nozzle diameter is: 0.6mm; Nozzle to the curing distance of accepting screen is: 13 ~ 15cm; Indoor temperature is: 15 ~ 20
oC; Relative humidity is: 45% ~ 60%.
Three, preparation ZnO/Ag composite nano fiber
With [PEG+PVP] that obtained/[Zn (NO
3)
2+ AgNO
3] composite nano fiber heat-treats, technical parameter is: heating rate is 1 ~ 2
oC/min is 500 ~ 800
oInsulation 2 ~ 5h in the C temperature range is with 1
oThe rate of temperature fall of C/min cools to 200
oNaturally reduce to room temperature during C, so far obtain the ZnO/Ag composite nano fiber.
Four, air-sensitive performance test
The nano-composite fiber that makes is ground, add small amount of deionized water furnishing pasty state then, evenly be coated with and be attached on the alumina ceramic tube; Earthenware is placed 600
oC Muffle furnace sintering 1h processes tube core, welding, and assembled formation, aging, at last 200
oC carries out the test of gas air-sensitive performance.
Prepared [PEG+PVP]/[Zn (NO in said process
3)
2+ AgNO
3] the composite nano fiber surface ratio is than smooth, prepared ZnO/Ag composite nano fiber is made up of nano particle.
The present invention is through the coating to prepared ZnO/Ag nano grain surface; Make it in the polymer of intending spinning, good stable dispersion property arranged; The main selection directly coats the nano particle for preparing with the low surfactant of plan spinning polymer molecular weight; Select the little polyvinylpyrrolidone (PVP) of molecular weight among the present invention, also alleviate the direct agglomeration traits of particle simultaneously; The fibre diameter that spins acquisition through static is even, and diameter is also more tiny.
Compare other preparation methods, the present invention has the following advantages:
(1) technology of the present invention is simple, cost is low, has improved the uniformity of ZnO/Ag nano particle dispersed and gained fiber in polymer solution.
(2) aspect doping, this preparation method mixes more easily, has solved the difficult problem of mixing to a certain extent.
(3) the nano particle composite fibre granule content of gained of the present invention is high, and fiber is long, has bigger specific area, at aspects such as gas sensor, photocatalysis, has a good application prospect.
Description of drawings
Fig. 1 is the XRD figure of ZnO fiber in the instance one of the present invention, from figure, can find out ZnO nano particle well-crystallized;
Fig. 2 is ZnO/Ag nano particle composite fibre sem photograph in the instance two of the present invention, from figure, can find out composite fibre surface smoother;
Fig. 3 is ZnO/Ag nano particle composite fibre XRD figure in the instance two of the present invention, from figure, can see the diffraction maximum of Ag;
Fig. 4 is the air-sensitive performance resolution chart of ZnO, ZnO/Ag (5 at%) and ZnO/Ag (10 at%) composite fibre of preparation in instance one, two of the present invention and the instance three; From figure, can find out obviously that the ZnO fibre air-sensitive characteristic behind the doping Ag is significantly improved, and the gas-sensitive property of ZnO/Ag (10 at%) composite fibre is higher than the air-sensitive performance of ZnO/Ag (5 at%).
The specific embodiment
Further specify content of the present invention below in conjunction with instance.
Instance one: Ag content is the nano particle composite fibre of 0atom %
With 4g Zn (NO
3)
26H
2O and 1gPVP add the 10ml deionized water respectively and the 10ml absolute ethyl alcohol and stirring is even; Mix then and stir 30min; 2gPEG is added the 20ml absolute ethyl alcohol and stirring; Add above-mentioned mixed solution, after the room temperature lower magnetic force stirs 6h, leave standstill 4h, can obtain homogeneous, transparent and [PEG+PVP]/Zn (NO of certain viscosity arranged
3)
2Spinning solution; The weight proportion of each part of this spinning solution is: Zn (NO
3)
26H
2O/ [PEG+PVP]/absolute ethyl alcohol/deionized water=4:3:30:10; The spinning solution that configures is added in the existing electrostatic spinning apparatus of device for spinning, carry out electrostatic spinning, nozzle diameter is 0.6mm, and operating voltage is 15kV; The syringe needle nozzle is 13cm to the curing distance of accepting screen; Indoor temperature is 15
oC, relative humidity is 45%, obtains [PEG+PVP]/Zn (NO
3)
2Composite nano fiber; With prepared [PEG+PVP]/Zn (NO
3)
2Composite nano fiber is put in the temperature programmed control stove and heat-treats, and heating rate is 1
oC/min is 520
oC constant temperature 2h, rate of temperature fall are 1
oC/min cools to 200
oNaturally reduce to room temperature during C, promptly obtain the ZnO nanofiber.
The nano-composite fiber that makes is ground, add small amount of deionized water furnishing pasty state then, evenly be coated with and be attached on the alumina ceramic tube, earthenware is placed 600
oC Muffle furnace sintering 1h processes tube core, welding, and assembled formation, aging, at last 200
oC carries out the test of gas air-sensitive performance.
Instance two: Ag content is the nano particle composite fibre of 5atom %
With 3.886g Zn (NO
3)
26H
2O and 0.114g AgNO
3Mix; It is even to add the 10ml deionized water and stirring; 1gPVP and 2gPEG are used the absolute ethyl alcohol of 10ml and the anhydrous alcohol solution of 20ml respectively; Then above-mentioned solution is mixed, after the room temperature lower magnetic force stirs 6h, leave standstill 4h, can obtain homogeneous, grey and [PEG+PVP]/[Zn (NO of certain viscosity is arranged
3)
2+ AgNO
3] spinning solution; The weight proportion of each part of this spinning solution is: [Zn (NO
3)
26H
2O+ AgNO
3]/[PEG+PVP)/absolute ethyl alcohol/deionized water=4:3:30:10, wherein AgNO
3With Zn (NO
3)
26H
2The amount of substance of O is than being 0.05:1; The spinning solution that configures is added in the existing electrostatic spinning apparatus of device for spinning, carry out electrostatic spinning, nozzle diameter is 0.6mm, and operating voltage is 15kV; The syringe needle nozzle is 13cm to the curing distance of accepting screen; Indoor temperature is 15
oC, relative humidity is 45%, obtains [PEG+PVP]/[Zn (NO
3)
2+ AgNO
3] composite nano fiber, Fig. 2 is the sem photograph of composite fibre, as can be seen from the figure composite fibre surface smoother.
With prepared [PEG+PVP]/[Zn (NO
3)
2+ AgNO
3] composite nano fiber is put in the temperature programmed control stove and heat-treats, heating rate is 1
oC/min is 520
oC constant temperature 2h, rate of temperature fall are 1
oC/min cools to 200
oNaturally reduce to room temperature during C, promptly obtain ZnO/Ag particle nanofiber.
Fig. 3 is the compound XRD figure of ZnO/Ag, and as can be seen from the figure at the ZnO/Ag composite fibre, the ZnO structure does not change, and has occurred the diffraction maximum of 2 silver-colored particles in the curve, and what they were corresponding respectively is Ag (111) and (200) crystal face.
The ZnO/Ag particle nano-composite fiber that makes is ground, add small amount of deionized water furnishing pasty state then, evenly be coated with and be attached on the alumina ceramic tube.Earthenware is placed 600
oC Muffle furnace sintering 1h processes tube core, welding, and assembled formation, aging, at last 200
oC carries out the test of gas air-sensitive performance.
Instance three: Ag content is the nano particle composite fibre of 10atom %
With 3.772g Zn (NO
3)
26H
2O and 0.228g AgNO
3Mix; It is even to add the 10ml deionized water and stirring; 1gPVP and 2gPEG are used the absolute ethyl alcohol of 10ml and the anhydrous alcohol solution of 20ml respectively; Then above-mentioned solution is mixed, after the room temperature lower magnetic force stirs 6h, leave standstill 4h, can obtain homogeneous, grey and [PEG+PVP]/[Zn (NO of certain viscosity is arranged
3)
2+ AgNO
3] spinning solution; The weight proportion of each part of this spinning solution is: [Zn (NO
3)
26H
2O+ AgNO
3]/[PEG+PVP]/absolute ethyl alcohol/deionized water=4:3:30:10, wherein AgNO
3With Zn (NO
3)
26H
2The amount of substance of O is than being 0.1:1; The spinning solution that configures is added in the existing electrostatic spinning apparatus of device for spinning, carry out electrostatic spinning, nozzle diameter is 0.6mm, and operating voltage is 15kV; The syringe needle nozzle is 13cm to the curing distance of accepting screen; Indoor temperature is 15
oC, relative humidity is 45%, obtains [PEG+PVP]/[Zn (NO
3)
2+ AgNO
3] composite nano fiber.
With prepared [PEG+PVP]/[Zn (NO
3)
2+ AgNO
3] composite nano fiber is put in the temperature programmed control stove and heat-treats, heating rate is 1
oC/min is 520
oC constant temperature 2h, rate of temperature fall are 1
oC/min cools to 200
oNaturally reduce to room temperature during C, promptly obtain ZnO/Ag particle nanofiber.
The ZnO/Ag particle nano-composite fiber that makes is ground, add small amount of deionized water furnishing pasty state then, evenly be coated with and be attached on the alumina ceramic tube, earthenware is placed 600
oC Muffle furnace sintering 1h processes tube core, welding, and assembled formation, aging, at last 200
oC carries out the test of gas air-sensitive performance.
Claims (1)
1. the preparation method of polyethylene glycol/ZnO/Ag nano particle complex fiber material comprises the steps:
(1) preparing spinning solution
What used in the zinc source in the spinning solution is zinc salt, is [Zn (NO
3)
26H
2O]; That use in the silver source is silver nitrate [AgNO
3]; High polymer templates adopts the mixture of polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP); Solvent adopts absolute ethyl alcohol and deionized water;
Take by weighing polyethylene glycol and polyvinylpyrrolidone and be dissolved in the absolute ethyl alcohol, mix again with through the zinc nitrate hexahydrate of ultrasonic dissolution and the mixed aqueous solution of silver nitrate, stir 4 ~ 10 h in the room temperature lower magnetic force, and leave standstill 2 ~ 6 h, promptly form spinning solution; The mass ratio of this each part of spinning solution is: [Zn (NO
3)
26H
2O+ AgNO
3]/[PEG+PVP]/absolute ethyl alcohol/deionized water=4:3:30:10, wherein the mass ratio of PEG and PVP is 2:1, AgNO
3With Zn (NO
3)
26H
2The amount of substance ratio of O is 0 ~ 0.1:1;
(2) preparation [PEG+PVP]/[Zn (NO
3)
2+ AgNO
3] composite nano fiber
Adopt electrostatic spinning technique, technical parameter is: DC voltage is: 15 ~ 20kV; The syringe needle nozzle diameter is: 0.6mm; Nozzle to the curing distance of accepting screen is: 13 ~ 15cm; Indoor temperature is: 15 ~ 20
oC; Relative humidity is: 45% ~ 60%;
(3) preparation ZnO/Ag composite nano fiber
With [PEG+PVP] that obtained/[Zn (NO
3)
2+ AgNO
3] composite nano fiber heat-treats, technical parameter is: heating rate is 1 ~ 2
oC/min is 500 ~ 800
oInsulation 2 ~ 5h in the C temperature range is with 1
oThe rate of temperature fall of C/min cools to 200
oNaturally reduce to room temperature during C, so far obtain the ZnO/Ag composite nano fiber.
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Cited By (6)
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| CN104931562A (en) * | 2015-05-11 | 2015-09-23 | 浙江理工大学 | Preparation method of FTO (Fluorine-doped Tin Oxide)-ZnO/CuO electrode |
| CN105823799A (en) * | 2016-03-22 | 2016-08-03 | 苏州捷德瑞精密机械有限公司 | Semiconductor gas-sensitive base material and preparation method thereof |
| CN106192077A (en) * | 2016-07-15 | 2016-12-07 | 宁波工程学院 | A kind of preparation method of Ag loading ZnO full meso-porous nano fiber |
| CN106367955A (en) * | 2016-09-22 | 2017-02-01 | 金陵科技学院 | Preparation method of nanoparticle composite electrospinning fiber with PH sensitive characteristics |
| CN107180702A (en) * | 2017-04-26 | 2017-09-19 | 浙江理工大学 | Silver/zirconium oxide/carbon composite nano-fiber membrane material, preparation method and application |
| CN113512313A (en) * | 2021-08-04 | 2021-10-19 | 青岛金芳华新型建材科技有限公司 | Waterproof and mildewproof composite coating and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931562A (en) * | 2015-05-11 | 2015-09-23 | 浙江理工大学 | Preparation method of FTO (Fluorine-doped Tin Oxide)-ZnO/CuO electrode |
| CN105823799A (en) * | 2016-03-22 | 2016-08-03 | 苏州捷德瑞精密机械有限公司 | Semiconductor gas-sensitive base material and preparation method thereof |
| CN106192077A (en) * | 2016-07-15 | 2016-12-07 | 宁波工程学院 | A kind of preparation method of Ag loading ZnO full meso-porous nano fiber |
| CN106367955A (en) * | 2016-09-22 | 2017-02-01 | 金陵科技学院 | Preparation method of nanoparticle composite electrospinning fiber with PH sensitive characteristics |
| CN107180702A (en) * | 2017-04-26 | 2017-09-19 | 浙江理工大学 | Silver/zirconium oxide/carbon composite nano-fiber membrane material, preparation method and application |
| CN113512313A (en) * | 2021-08-04 | 2021-10-19 | 青岛金芳华新型建材科技有限公司 | Waterproof and mildewproof composite coating and preparation method thereof |
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