CN100595355C - Method for preparing coaxial compound nano thread of monocrystal zinc oxide wrapped by organic polymer - Google Patents
Method for preparing coaxial compound nano thread of monocrystal zinc oxide wrapped by organic polymer Download PDFInfo
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- CN100595355C CN100595355C CN200710025524A CN200710025524A CN100595355C CN 100595355 C CN100595355 C CN 100595355C CN 200710025524 A CN200710025524 A CN 200710025524A CN 200710025524 A CN200710025524 A CN 200710025524A CN 100595355 C CN100595355 C CN 100595355C
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Abstract
The present invention relates to a method for preparing organic polymer enveloped monocrystal zinc oxide coaxial composite nano wire. Said method includes the following steps: (1), preparing monocrystal zinc oxide nano wire; (2), preparing mixed solution of polymer and zinc oxide; and (3), preparing coaxial composite structure of monocrystal zinc oxide nano wire enveloped by polymer. Said invention can be used for making various nano function devices.
Description
Technical field
The present invention relates to a kind of electronic fiber---the preparation method of organic polymer and semiconductor monocrystal coaxial compound nano is a kind of gas phase transmission method prepares the coaxial composite construction of nano wire of thread of monocrystal zinc oxide wrapped by organic polymer in conjunction with electrostatic spinning a method.
Background technology
Nano material's structure and pattern have very big influence to the performance and the application of nano material.The nano crystal material of ad hoc structure and pattern has important meaning for the frontier of exploitation nano material application function.Recently, the one dimension semiconductor material is studied extensively and profoundly, mainly pays close attention to its monocrystalline (high electron mobility) and one-way, and can go up at inorganization substrate (the not strict coupling of lattice) and collect the growth of living.Therefore, they are expected to become high-performance (near single crystal device) large area electron or the good substitute of opto-electronic device.However, directly these nano wires of large area deposition are very difficult on a substrate that designs pattern, and these nano wires are distributed on the large-area substrate in the mode that is arranged in parallel also is a huge challenge.Though there is certain methods that they are arranged in parallel, such as liquid aggregation method and electrophoresis, its uniformity also remains a problem, especially is evenly distributed in the large tracts of land scope.In this patent, we have designed a kind of method and have prepared electronic fiber, the coaxial composite fibre of promptly a kind of insulating materials (plastics or inorganic matter) parcel semiconductor nanowires.This electronic fiber can be made scroll as optical fiber, can be printed or be compressed on almost any substrate and make device or system.In principle, such device can have this semiconductor due key property (such as the performance of body monocrystal material).We will explain the notion of this electronic fiber as representative with ZnO in the following literal.
In numerous nano materials, nanometer semiconductor structure has caused people's extensive concern, and the general especially interested research and development focus of the nanostructured of zinc oxide.Zinc oxide is a kind of 60meV of having exciton bind energy and the wide direct band-gap semicondictor of 3.37eV.The zinc oxide of nanostructured enjoys attention owing to its bigger surface area and good light, electricity, magnetic property, and it is expected in fields such as biology sensor, gas sensor, storage hydrogen device, metal-ion battery, electric chemical super electric capacity, photocell, FPD good application prospects is arranged.
At present, method of electrostatic spinning is a kind of multiple method at the organic polymer nanofiber of preparation that is widely used in, also there are many people to use this method to carry out the preparation of zinc oxide nano fiber, but with other chemical method, compare as gas phase transmission method, pyrolysis method, hydrothermal decomposition method or the like, the zinc oxide nano fiber crystallinity that electrostatic spinning obtains is relatively poor relatively, is difficult to form mono-crystalline structures.Also there is same problem in the composite nano fiber preparation of zinc oxide and other organic polymer.Therefore work out a kind of easy to operate, output is abundant, crystalline nature is good, and the coaxial composite nanostructure preparation method of the nanometer monocrystalline zinc oxide line of even structure and polymer all has significance to developing new material and further developing the novel nano function element.
Summary of the invention
The method of technical problem: the purpose of this invention is to provide a kind of electronic fiber for preparing even structure---organic polymer and the coaxial composite nanostructure of single-crystal zinc-oxide nano line.This method has been simplified experimental rig, greatly reduces with polymer and zinc acetate mixed solution to carry out the difficulty that electrostatic spinning obtains coaxial composite fibre.In the organic matter parcel zinc oxide compound nano line that obtains among the present invention, zinc oxide nanowire is the monocrystalline attitude, have good photoelectric characteristic, be more conducive to make the photoelectric device of various superior performances, thereby provide more nimble space for the design of novel nano photoelectric functional device.
Technical scheme: the present invention is a kind of method for preparing coaxial compound nano thread of monocrystal zinc oxide wrapped by organic polymer:
Preparation method of the present invention comprises the steps:
Step 1: preparation single-crystal zinc-oxide nano line: with silicon, sapphire or quartzy in the middle of any be substrate, with oxygen and argon gas as carrier gas, with zinc powder as raw material under 600-750 ℃ of condition, or be raw material with the mixture of Zinc oxide powder and carbon dust, under 1050-1150 ℃, the constant 0.09MPa condition of air pressure, reacted 30 minutes, and obtained the single-crystal zinc-oxide nano line;
Step 2: the mixed solution of preparation polymer and zinc oxide: with the single-crystal zinc-oxide nano line that obtains in the step 1, sneak in the polymer solution that has prepared, obtain the mixed solution of homogeneous polymer and zinc oxide through stirring;
Step 3: the coaxial composite construction of preparation polymer thread of monocrystal zinc oxide wrapped nano wire: with the polymer that obtains in the step 2 and the mixed solution of zinc oxide, carry out electrostatic spinning, obtain the coaxial composite construction of polymer thread of monocrystal zinc oxide wrapped nano wire, zinc oxide is the monocrystalline attitude in the coaxial composite nanostructure that is obtained.
Aerating oxygen and argon gas volume ratio are 1: 20 in preparation method's step 1 of the present invention, polymer solution is any in polyvinyl alcohol, polymethyl-benzene olefin(e) acid second fat, silicon rubber, the polystyrene in the step 2, and single-crystal zinc-oxide nano line and polymer solution mass ratio are between 1: 20 to 1: 40.
Beneficial effect: compared with prior art, the present invention has following advantage:
1. the technology of preparing of two kinds of method nanofibers has been merged in the present invention, is used for obtaining the coaxial composite nanostructure of organic polymer thing and single-crystal zinc-oxide nano line.By the first preparation nanometer monocrystalline zinc oxide line of gas phase transmission method, guaranteed the good crystallinity of zinc oxide nanowire in the composite nano-line of method of electrostatic spinning preparation.As long as just can obtain coaxial nanostructured with common electrostatic spinning apparatus, simplified experimental rig, greatly reduce with polymer and zinc acetate mixed solution and carry out the difficulty that electrostatic spinning obtains coaxial composite fibre.
2. in the organic matter parcel zinc oxide compound nano line that the present invention obtains, zinc oxide nanowire is the monocrystalline attitude, has good photoelectric characteristic, be more conducive to make the photoelectric device of various superior performances, as the FET in the large area electron device (active array among the LCD or the like), chemical/biological sensors and feds etc.
3. can be among the present invention by the photoelectric characteristic of the reasonable controlled material of composition adjustment of polymer and nano wire in the coaxial composite nanostructure preparation process of organic polymer thing and single-crystal zinc-oxide nano line, thus more nimble space provided for the design of novel nano photoelectric functional device.
Description of drawings
Fig. 1 is the experimental provision schematic diagram that the gas phase transmission method prepares zinc oxide nanowire.Wherein have: find time mouth 1, alundum tube 2, silicon substrate 3, quartz ampoule 4, raw material 5, carrier gas 6.
Fig. 2 is scanning electron microscopy (SEM) image of the zinc oxide nanowire that prepared by the present invention.
Fig. 3 is the experimental provision schematic diagram that method of electrostatic spinning prepares the thread of monocrystal zinc oxide wrapped by organic polymer composite nano fiber.Wherein have: high voltage source 1, electrostatic spinning solution 2, syringe 3, receiving system 4.
Fig. 4 is scanning electron microscopy (SEM) image (side view) of the PVA nanofiber that prepared by the present invention.
Fig. 5 is the structural representation that is wrapped up the single crystal semiconductor coaxial compound nano by the polymer that the present invention obtains.
The specific embodiment
Be that specific embodiments of the invention further describe below:
Embodiment one:
The first step: with the silicon chip is substrate, mixture with zinc oxide and carbon dust in the tube furnace of controllable temperature is that raw material are under 1150 ℃ of conditions, feed volume ratio and be 1: 20 oxygen and argon gas as carrier gas, holding tube internal gas pressure 0.09MPa, reacted 30 minutes, concrete course of reaction in Fig. 1, find time from alundum tube (2) left side of moderate oven mouthful (1) find time, be in Zn steam that the raw material (5) in relatively-high temperature district produce under the transportation of alundum tube (2) the right side carrier gas (6) of moderate oven to the motion of substrate direction, be on silicon substrate (3) quartz ampoule (4) of relative low-temperature region and will grow the single-crystal zinc-oxide nano line.
Second step: the single-crystal zinc-oxide nano line that the first step is obtained scrapes from substrate, mixes at 1: 30 by mass ratio with 9% poly-vinyl alcohol solution (PVA) that has prepared, stirs and obtains the homogeneous mixed liquor in 10 hours.
The 3rd step: in Fig. 3, electrostatic spinning solution (2) threading is had in the syringe (3) of capillary shower nozzle, and the high voltage source (1) of 30KV in addition, thereby (spacing 15cm) sets up a powerful field of electric force between the receiving system of shower nozzle and ground connection, electric field force overcomes solution surface tension makes it to become jet, jet is producing stretching from spout to receiving system (4) motion process, finally form the nanofiber among Fig. 4,5 on receiving system.This fiber shows as the coaxial composite construction of polymer thread of monocrystal zinc oxide wrapped nano wire.
Embodiment two:
The first step: with silicon is substrate, in the tube furnace of controllable temperature with zinc powder as raw material under 700 ℃ of conditions, feed volume ratio and be 1: 20 oxygen and argon gas as carrier gas, the constant 0.09MPa of holding tube internal gas pressure, reacted 30 minutes, be in Zn steam that the raw material in relatively-high temperature district produce under the transportation of carrier gas to the motion of substrate direction, be on the substrate of relative low-temperature region and will grow the single-crystal zinc-oxide nano line.
Second step: the single-crystal zinc-oxide nano line that the first step is obtained scrapes from substrate, and 9% polyvinyl alcohol (PVA) solution with having prepared mixes by mass ratio at 1: 20, stirs and obtains the homogeneous mixed liquor in 10 hours.
The 3rd step: the mixed solution threading of polymer and zinc oxide is had in the syringe of capillary shower nozzle, and add the high pressure of 25KV, thereby (spacing 10cm) sets up a powerful field of electric force between the receiving system of shower nozzle and ground connection, electric field force overcomes solution surface tension makes it to become jet, jet is producing stretching from spout to the receiving system motion process, finally form nanofiber on receiving system.
Embodiment three:
The first step: with the silicon chip is substrate, mixture with zinc oxide and carbon dust in the tube furnace of controllable temperature is that raw material are under 1050 ℃ of conditions, feed volume ratio and be 1: 30 oxygen and argon gas as carrier gas, holding tube internal gas pressure 0.09MPa reacts and will obtain the single-crystal zinc-oxide nano line in 30 minutes.
Second step: the single-crystal zinc-oxide nano line that the first step is obtained scrapes from substrate, mixes at 1: 40 by mass ratio with 9% poly-vinyl alcohol solution (PVA) that has prepared, stirs and obtains the homogeneous mixed liquor.
The 3rd step: the mixed solution threading of polymer and zinc oxide is had in the syringe of capillary shower nozzle, and the high pressure of 28KV in addition, thereby to the receiving system motion process, producing stretching from spout at (spacing 12cm) jet between the receiving system of shower nozzle and ground connection, finally on receiving system, forming nanofiber.
Claims (4)
1. the method for preparing coaxial compound nano thread of monocrystal zinc oxide wrapped by organic polymer is characterized in that this method comprises the steps:
Step 1. preparation single-crystal zinc-oxide nano line: with silicon, sapphire or quartzy in the middle of any be substrate, with oxygen and argon gas as carrier gas, with zinc powder as raw material under 600-750 ℃ of condition, under the constant 0.09MPa condition of air pressure, reacted 30 minutes, and obtained the single-crystal zinc-oxide nano line;
Step 2. the mixed solution of preparation polymer and zinc oxide: with the single-crystal zinc-oxide nano line that obtains in the step 1, sneak in the polymer solution that has prepared, single-crystal zinc-oxide nano line and polymer solution mass ratio are 1: 20-40 obtains the mixed solution of homogeneous polymer and zinc oxide through stirring;
Step 3. the coaxial composite construction of preparation polymer thread of monocrystal zinc oxide wrapped nano wire: with the polymer that obtains in the step 2 and the mixed solution of zinc oxide, carry out electrostatic spinning, obtain the coaxial composite construction of polymer thread of monocrystal zinc oxide wrapped nano wire, zinc oxide is the monocrystalline attitude in the coaxial composite nanostructure that is obtained.
2. the method for preparing the polymer coaxial compound nano thread of monocrystal zinc oxide wrapped as claimed in claim 1, it is characterized in that in step 1, with the mixture of Zinc oxide powder and carbon dust is raw material under 1050-1150 ℃, the constant 0.09MPa condition of air pressure, reacted 30 minutes, and obtained the single-crystal zinc-oxide nano line.
3. the method for preparing the polymer coaxial compound nano thread of monocrystal zinc oxide wrapped as claimed in claim 1 is characterized in that aerating oxygen and argon gas volume ratio are 1: 20 in the step 1.
4. the method for preparing the polymer coaxial compound nano thread of monocrystal zinc oxide wrapped as claimed in claim 1 is characterized in that polymer solution in the step 2 is any in polyvinyl alcohol, polymethyl-benzene olefin(e) acid second fat, silicon rubber, the polystyrene.
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| CN101735632B (en) * | 2008-11-26 | 2012-05-30 | 清华大学 | Nano composite particle and preparation method thereof |
| US9148969B2 (en) * | 2012-07-30 | 2015-09-29 | Rohm And Haas Electronic Materials Llc | Method of manufacturing high aspect ratio silver nanowires |
| EP3406675A1 (en) * | 2017-05-22 | 2018-11-28 | InnovationLab GmbH | Electronic and optoelectronic devices having anisotropic properties and method for their production |
| CN107478680B (en) * | 2017-08-06 | 2018-11-23 | 江苏来德福汽车部件有限公司 | A kind of harmful gas in vehicle detection device |
| CN107315036A (en) * | 2017-08-06 | 2017-11-03 | 潘金文 | One kind is based on SnO2The alcohol gas sensor of composite nano fiber |
| CN113353969B (en) * | 2021-06-29 | 2023-07-04 | 科迈特新材料有限公司 | Preparation method of high-activity nano zinc oxide |
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| 无机功能性纳米材料与高分子纳米纤维的复合. 柳巍.中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑，第04期. 2004 |
| 无机功能性纳米材料与高分子纳米纤维的复合. 柳巍.中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑，第04期. 2004 * |
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