CN102851791A - Preparation method of high-conductivity high-wide-spectrum-permeability MgZnAlO and nano-fiber of composite structure thereof - Google Patents
Preparation method of high-conductivity high-wide-spectrum-permeability MgZnAlO and nano-fiber of composite structure thereof Download PDFInfo
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- CN102851791A CN102851791A CN2012101766767A CN201210176676A CN102851791A CN 102851791 A CN102851791 A CN 102851791A CN 2012101766767 A CN2012101766767 A CN 2012101766767A CN 201210176676 A CN201210176676 A CN 201210176676A CN 102851791 A CN102851791 A CN 102851791A
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Abstract
The invention relates to an electro-spinning and atomic layer deposition composite technology used for preparing high-conductivity high-wide-spectrum-permeability MgZnAlO and nano-fiber of composite structure thereof. The method comprises the three steps that: 1, PVP nano-fiber is grown by using the electro-spinning technology; 2, the PVP nano-fiber is adopted as a template, and an MgZnAlO thin layer is deposited on the template with the atomic layer deposition technology, such that MgZnAlO/PVP composite structure nano-fiber is constructed; and 3, the composite structure fiber is subjected to a high-temperature annealing treatment, such that PVP is removed, and MgZnAlO nano-fiber is obtained. According to the invention, MgZnAlO/PVP composite structure nano-fiber with different components and different diameters can be obtained by changing parameters in the deposition process. The obtained fiber has good toughness, good strength, high conductivity, smooth surface structure, and high permeability to wide spectrum. Component controls can be carried out upon the doped Mg and Al according to requirements.
Description
Technical field
The present invention relates to the method for the nanofiber preparation of a kind of MgZnAlO and composite construction thereof, be method growth high conductivity, the MgZnAlO of wide spectrum high-permeability and the nanofiber of composite construction thereof that utilizes electrostatic spinning technique and technique for atomic layer deposition to combine, belong to technical field of semiconductor.
Background technology
Nanofiber has many excellent properties, such as the brass speculum, placed in the sun to generate enough heat to ignite dry gass channel effect of small-size effect, surface and interface effect, quantum size effect macroscopic quantum, thereby all have a wide range of applications in various fields such as chemical industry, medicine, coating, auto industry, bioengineering and photocatalysis.Nanofiber comprises inorganic nano-fiber and organic nanofibers.The method of grown nanofibers has much at present, such as extension, template synthetic method, self-assembly method, microphase-separated method and electrostatic spinning etc.Wherein electrostatic spinning technique is with simple to operate, applied widely, production efficiency advantages of higher and being widely used relatively.But for inorganic nano-fiber, when preparation electrospinning solution, at first need and will inorganic salts be added in the organic polymer solvent, its dissolution degree will greatly affect the last pattern of product.And when the preparation inorfil, need carry out high-temperature process, remove the organic principle in the fiber, the inorganic nano-fiber majority that therefore obtains all is that polycrystalline particle consists of, and it is rough, presents a chain or loose structure more.In addition, in carrying out the nanofiber preparation process of multicomponent alloy, the control of its component is also comparatively difficult.Therefore need to there be more outstanding preparation means or method to address the above problem.
The energy gap of ZnO is 3.37eV, and exciton bind energy 60meV has the high and outstanding room temperature luminous performance of transparency, and is ep-type material, abundant raw material, and cost is low, and is nontoxic.At rubber manufacturing, ceramic industry, medical and health, electronic applications, cosmetic field application is arranged, particularly in the products such as the liquid crystal display of semiconductor applications, thin film transistor (TFT), light emitting diode, have a wide range of applications.And nano-ZnO is owing to have the distinctive character of nano material so that it has showed very wide, tempting prospect in fields such as space flight, electronics, metallurgy, chemistry, biology and environmental protection.Yet along with going deep into of research, require material to have better conductive characteristic, wider spectrum permeability, so continual exploitation has the nano-fiber material of These characteristics.
Summary of the invention
For the problem that proposes in the background technology, the method that the present invention has adopted electrostatic spinning technique and ald (ALD) technology to combine prepares the MgZnAlO of high conductivity, wide spectrum high-permeability and the nanofiber of composite construction thereof, method is simple, realize easily the nanofiber that obtains.
Concrete steps of the present invention are:
1. adopt electrostatic spinning technique growth PVP nanofiber.
With the PVP nanofiber as template, utilize technique for atomic layer deposition to deposit the MgZnAlO thin layer thereon, make up MgZnAlO/PVP composite construction nanofiber.
3. the composite construction nanofiber is carried out the high temperature anneal, can remove the PVP template, obtain tubulose MgZnAlO nanofiber.
Its technique effect of the present invention is, in conjunction with electrostatic spinning technique and ald (ALD) technology, and resulting nanofiber smooth surface, and can accurately control fiber size and chemical constituent.As shown in Figure 1.By the adjusting to Mg and Al component, obtain the nanofiber of high conductivity, wide spectrum high-permeability.
Description of drawings
Fig. 1 is the SEM image of the MgZnAlO/PVP composite construction nanofiber of embodiment one acquisition.Fig. 2 is the EDS spectrum of the MgZnAlO/PVP composite construction nanofiber of example one acquisition.Fig. 1 doubles as and is Figure of abstract.
The specific embodiment
Embodiment one:
1, preparation PVP electrospinning solution adopts electrostatic spinning technique growth PVP nanofiber, and growth process is as follows:
(1) forms the PVP/ ethanolic solution in 10 milliliters of ethanol of the PVP of 0.5g dissolving, then stirred 5 hours.Before the electrostatic spinning, solution is static the placement 24 hours in order to remove bubble at room temperature.
(2) precursor solution is packed into and is furnished with the syringe of syringe needle, and the positive pole of high voltage source (up to 30kv) is connected to syringe needle, and negative pole is connected to the aluminium foil collecting board simultaneously.In this experiment, the high pressure that applies is that the distance of 10 kilovolts of while needle points and aluminium foil collecting board is 15 centimetres.The fiber of PVP just is collected on the aluminium foil collecting board.
2, take PVP as template, deionized water, diethyl zinc, trimethyl aluminium and ethyl diamyl magnesium are precursor source, adopt technique for atomic layer deposition deposition MgZnAlO thin layer, obtain MgZnAlO/PVP composite construction nanofiber, and growth course is as follows:
(1) burst length: four precursor source pulses are 15ms
(2) stand-by period: except the deionized water stand-by period is 5s, its excess-three precursor source stand-by period is respectively 5s, 5s and 5s.
(3) growth temperature: the temperature of ethyl diamyl magnesium is 80 ℃, and all the other precursor source temperature are that room temperature gets final product.Reaction chamber temperature is 150 ℃ and deposits;
(4) cycle period: deionized water, diethyl zinc carry out deposition 4 times, and deionized water, ethyl diamyl magnesium carry out deposition 1 time, circulate 4 times, and deionized water, trimethyl aluminium carry out deposition 1 time, circulate 2 times.Reaction obtains MgZnAlO/PVP composite construction nanofiber after finishing, as shown in Figure 1.
3, in the nanofiber of composite construction, carried out the high temperature anneal, when temperature reaches uniform temperature (about 400 ℃), just can remove the PVP template, obtain tubulose MgZnAlO nanofiber.
Embodiment two:
1, preparation PVP electrospinning solution adopts electrostatic spinning technique growth PVP nanofiber, and growth process is as follows:
(1) forms the PVP/ ethanolic solution in 10 milliliters of ethanol of the PVP of 0.5g dissolving, then stirred 5 hours.Before the electrostatic spinning, solution is static the placement 24 hours in order to remove bubble at room temperature.
(2) precursor solution is packed into and is furnished with the syringe of syringe needle, and the positive pole of high voltage source (up to 30kv) is connected to syringe needle, and negative pole is connected to the aluminium foil collecting board simultaneously.In this experiment, the high pressure that applies is that the distance of 10 kilovolts of while needle points and aluminium foil collecting board is 15 centimetres.The fiber of PVP just is collected on the aluminium foil collecting board.
2, take PVP as template, deionized water, diethyl zinc, trimethyl aluminium and ethyl diamyl magnesium are precursor source, adopt technique for atomic layer deposition deposition MgZnAlO thin layer, obtain MgZnAlO/PVP composite construction nanofiber, and growth course is as follows:
(1) burst length: four precursor source pulses are 20ms;
(2) stand-by period: except the deionized water stand-by period is 5s, its excess-three precursor source stand-by period is respectively 6s, 6s and 6s.
(3) growth temperature: the temperature of ethyl diamyl magnesium is 85 ℃, and all the other precursor source temperature are that room temperature gets final product.Reaction chamber temperature is 120 ℃ and deposits;
(4) cycle period: deionized water, diethyl zinc carry out deposition 5 times, and deionized water, ethyl diamyl magnesium carry out deposition 1 time, circulate 4 times, and deionized water, trimethyl aluminium carry out deposition 1 time, circulate 2 times.Reaction obtains MgZnAlO/PVP composite construction nanofiber after finishing, as shown in Figure 1.
3, in the nanofiber of composite construction, carried out the high temperature anneal, when temperature reaches uniform temperature (about 400 ℃), just can remove the PVP template, obtain tubulose MgZnAlO nanofiber.
Claims (6)
1. a method that combines with electrostatic spinning technique and technique for atomic layer deposition prepares the method for the nanofiber of the MgZnAlO of high conductivity, wide spectrum high-permeability and composite construction thereof, and the implementation step is:
(1) preparation electrospinning liquation adopts electrostatic spinning technique growth PVP nanofiber.
(2) take the PVP nanofiber as template, utilize technique for atomic layer deposition to deposit the MgZnAlO thin layer thereon, make up MgZnAlO/PVP composite construction nanofiber and MgZnAlO nanofiber.
(3) this method can accurately be controlled the diameter of fiber, and the nanofiber surface smoothing that obtains, size uniform.
(4) this method can be accurately controlled the Mg that mixes and the component of Al.
(5) the composite construction nanofiber is carried out the high temperature anneal, remove the PVP template, can obtain tubulose MgZnAlO nanofiber.
2. according to claim 1, the inventive method can prepare high conductivity, wide spectrum high-permeability nanofiber.
3. according to claim 1, the method that the present invention prepares nanofiber is characterised in that: the method growth MgZnAlO that combines with electrostatic spinning technique and technique for atomic layer deposition and the nanofiber of composite construction thereof.
4. according to claim 1, the present invention uses technique for atomic layer deposition, can be simply accurately according to the diameter of controlled circulation cycle at atomic level control nanofiber.
5. according to claim 1, the control to the component of the Mg that mixes and Al among the present invention also is fairly simple and accurate.Need only the content that each component just can be accurately controlled in the programming that changes in each component as required by calculating.
6. according to claim 1, the present invention preparation the MgZnAlO nanofiber be that the MgZnAlO/PVP composite nano fiber is directly carried out the high temperature anneal, remove the PVP template.
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WO2015035656A1 (en) * | 2013-09-16 | 2015-03-19 | Liu Juntao | Alarm clock |
CN104451955A (en) * | 2014-11-25 | 2015-03-25 | 中国科学院电子学研究所 | Metal or metal oxide with hierarchical structure and preparation method of metal or metal oxide |
CN106592197A (en) * | 2016-12-20 | 2017-04-26 | 大连交通大学 | Preparation method of multifunctional electrostatic spinning luminescent fiber with core-shell structure |
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WO2015035656A1 (en) * | 2013-09-16 | 2015-03-19 | Liu Juntao | Alarm clock |
CN104451955A (en) * | 2014-11-25 | 2015-03-25 | 中国科学院电子学研究所 | Metal or metal oxide with hierarchical structure and preparation method of metal or metal oxide |
CN106592197A (en) * | 2016-12-20 | 2017-04-26 | 大连交通大学 | Preparation method of multifunctional electrostatic spinning luminescent fiber with core-shell structure |
CN106592197B (en) * | 2016-12-20 | 2019-05-28 | 大连交通大学 | A kind of preparation method of the Multifunctional static electricity spinning luminescent fibre with core-shell structure |
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