CN105002598B - A kind of preparation method of ZnO meso-porous nanos fiber - Google Patents
A kind of preparation method of ZnO meso-porous nanos fiber Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of ZnO meso-porous nanos fiber, belong to technical field of semiconductor material preparation.The preparation method is：PVP/ZnAc/TS spinning liquid as precursor is prepared, by prepared spinning liquid as precursor after spinning obtains precursor nano wire, ZnO meso-porous nano fibers are obtained through high-temperature calcination.For the present invention using foaming auxiliary electrostatic spining technology, by regulating and controlling TS concentration preparation high-purity ZnO meso-porous nano fibers, and preparation process of the present invention is simple, reproducible.
Description
Technical field
Preparation method more particularly to a kind of preparation side of ZnO meso-porous nanos fiber the present invention relates to a kind of nanofiber
Method belongs to technical field of semiconductor material preparation.
PVP refers to polyvinylpyrrolidone in the present invention；TS refers to Tea Saponin；ZnAc refers to zinc acetate, including water-containing acetic acid zinc
Or acetic anhydride zinc；Circular either ellipse or circular or oval or bandlet shape or subcircular in bandlet shape
Either nearly ellipse or nearly bandlet shape include but not limited to positive round, smooth or rough subcircular, ellipse, it is smooth or
Rough nearly ellipse, flat belt-like, smooth either rough or tortuous squashed structure.
Background technology
It is extensive since monodimension nanometer material has the characteristics such as anisotropic, larger width-thickness ratio, higher specific surface area
How real it is applied to one of the every field such as photodetection, magnetic material, gas sensor, luminescence generated by light, key foundation
The preparation of the nano material of existing high quality and its structure regulating.
ZnO nano material has stable chemical property, unique optically and electrically characteristic, is subject to many scientific workers
Pro-gaze.It, can be exposed in fibrous external by atom or crystal grain to greatest extent especially into the ZnO nano material of meso-hole structure
And as surface atom, the skin effect of nano material is able to performance to a greater extent so that specific surface area is further
Increase, application prospect are also more wide.At present, the method for preparing ZnO meso-porous nano fibers mainly has physical vapour deposition (PVD)+high temperature
Oxidizing process, hot volatilization+high-temperature oxidation and hydro-thermal method etc..Although existing technology of preparing has been achieved for good achievement,
Still it is faced with preparation process complexity, material prepared purity is relatively low, pore size differs, yield is more low difficult and challenge.
The content of the invention
The purpose of the present invention is be directed to the above-mentioned problems in the prior art, it is proposed that a kind of preparation process is simply, again
Renaturation is good, purity is high, the preparation method of the measured ZnO meso-porous nanos fiber of matter.
The purpose of the present invention can be realized by following technical proposal：A kind of preparation method of ZnO meso-porous nanos fiber, should
Preparation method is：PVP/ZnAc/TS spinning liquid as precursor is prepared, prepared spinning liquid as precursor is obtained into precursor through spinning
After nano wire, ZnO meso-porous nano fibers are obtained through high-temperature calcination.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, PVP/ZnAc/TS spinning liquid as precursor is through electrostatic spinning
Precursor nano wire is obtained, the wherein voltage of electrostatic spinning is 12-13kV, and the distance between cathode and anode are 18-25cm.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, obtained precursor nano wire also passes through drying process
Carry out high-temperature calcination again afterwards, drying process is dried in the shade for low temperature drying or room temperature.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, low temperature drying is precursor nano wire at 50-80 DEG C
Drying process when progress 8-14 is small.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, it is precursor nano wire in room temperature condition that room temperature, which is dried in the shade,
When lower aeration-drying 16-24 is small, ventilation wind speed is 1-2m/s.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, PVP/ZnAc/TS spinning liquid as precursor is configured to will be suitable
Amount PVP is dissolved in ethyl alcohol, and stirring at normal temperature obtains transparent and homogeneous solution, then adds in zinc acetate, water and TS, then heating water bath obtains
To yellow PVP/ZnAc/TS spinning liquid as precursor.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, ethyl alcohol when PVP/ZnAc/TS spinning liquid as precursor configures
Mass ratio with water is (3-1)：1, wherein water is deionized water or distilled water.By controlling water and second in precursor solution
The content of alcohol realizes the accurate control of organic precursor monodimension nanometer material structure.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, PVP/ZnAc/TS spinning liquid as precursor is every when configuring
1gPVP is dissolved in 3-9g ethyl alcohol.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, spinning when PVP/ZnAc/TS spinning liquid as precursor configures
In liquid often containing 1gPVP then ZnAc usage amount be 2-5g.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, spinning when PVP/ZnAc/TS spinning liquid as precursor configures
Often containing 1gPVP, then TS usage amounts are 0.01-1g in liquid.
In the preparation method of above-mentioned ZnO meso-porous nano fibers, high-temperature calcination is to be protected at 300-480 DEG C of calcining heat
Temperature calcining 1-3h, heating rate is 2-4 DEG C/min during calcining.
Method of electrostatic spinning is simple for process, fiber morphology is controllable, of low cost, be prepare fibrous material main path it
One.The present invention is then mesoporous by regulating and controlling TS concentration preparation high-purity ZnO by being improved and optimizing to electrostatic spinning technique
Nanofiber realizes the controllable preparation of the ZnO meso-porous nano fibers of high-purity.
The ZnO meso-porous nano fibers component that the above-mentioned preparation method of the present invention is prepared is Zn, O and other can not keep away
The impurity element exempted from,
Nanofiber has porous structure, and the hole of porous structure is including mesoporous；
Wherein main forms of Zn, O element in nanofiber are that (ZnO crystalline structures in nano wire are six to ZnO
Side wurtzite structure either cubic sphalerite structure) nanofiber is being circular or oval perpendicular to growth axis normal section
Shape either bandlet shape or subcircular or nearly ellipse or nearly bandlet shape.
A kind of improvement of ZnO meso-porous nanos fiber disclosed by the invention has the specific surface of the nanofiber of meso-hole structure
Product is 45-55m2/ g, mesoporous aperture averaging are 3-20nm.
Compared with prior art, the present invention has the advantages that following：
1. the present invention prepares high-purity ZnO meso-porous nanos using foaming auxiliary electrostatic spining technology by regulating and controlling TS concentration
Fiber.
2. the preparation process of high-purity ZnO meso-porous nano fibers of the present invention is simple, reproducible.
Description of the drawings
Scanning electron microscope (SEM) photograph under the low resolution multiplying power of solid-state precursor nano wires of the Fig. 1 obtained by the embodiment of the present invention 1.
Fig. 2 is the solid-state precursor nano wire cross-sectional scans electron microscope obtained by the embodiment of the present invention 1.
Fig. 3, which is that the ZnO meso-porous nano fibers obtained by the embodiment of the present invention 1 are low, differentiates scanning electron microscope (SEM) photograph under multiplying power.
Fig. 4 is the single ZnO meso-porous nanos fiber scanning electron microscope (SEM) photograph obtained by the embodiment of the present invention 1.
Fig. 5 is the single ZnO meso-porous nanos fibre section scanning electron microscope (SEM) photograph obtained by the embodiment of the present invention 1.
Fig. 6 is the ZnO meso-porous nano fiber X-ray diffracting spectrums obtained by the embodiment of the present invention 1.
Scanning electron microscope (SEM) photograph under the low resolution multiplying power of solid-state precursor nano wires of the Fig. 7 obtained by the embodiment of the present invention 2.
Fig. 8 is the scanning electron microscope (SEM) photograph in the single solid-state precursor nano wire section obtained by the embodiment of the present invention 2.
Fig. 9, which is that the ZnO meso-porous nano fibers obtained by the embodiment of the present invention 2 are low, differentiates scanning electron microscope (SEM) photograph under multiplying power.
Scanning electron microscope (SEM) photograph under ZnO meso-porous nano fiber high-resolution multiplying powers of the Figure 10 obtained by the embodiment of the present invention 2.
Figure 11 is the single ZnO meso-porous nanos fibre section scanning electron microscope (SEM) photograph obtained by the embodiment of the present invention 2.
Scanning electron microscope under the low resolution multiplying power of solid-state precursor nano-materials of the Figure 12 obtained by the embodiment of the present invention 3
Figure.
Figure 13 is the scanning electron microscope (SEM) photograph in the single solid-state precursor nano-material section obtained by the embodiment of the present invention 3.
Figure 14, which is that the ZnO meso-porous nano fibers obtained by the embodiment of the present invention 3 are low, differentiates scanning electron microscope (SEM) photograph under multiplying power.
Scanning electron microscope (SEM) photograph under ZnO meso-porous nano fiber high-resolution multiplying powers of the Figure 15 obtained by the embodiment of the present invention 3.
Figure 16 is the single ZnO meso-porous nanos fibre section scanning electron microscope (SEM) photograph obtained by the embodiment of the present invention 3.
Scanning electron microscope (SEM) photograph under the low resolution multiplying power of solid precursor nano wires of the Figure 17 obtained by the embodiment of the present invention 4.
Figure 18 is the scanning electron microscope (SEM) photograph in the single solid precursor nano wire section obtained by the embodiment of the present invention 4.
Figure 19, which is that the ZnO meso-porous nano fibers obtained by the embodiment of the present invention 4 are low, differentiates scanning electron microscope (SEM) photograph under multiplying power.
Scanning electron microscope (SEM) photograph under ZnO meso-porous nano fiber high-resolution multiplying powers of the Figure 20 obtained by the embodiment of the present invention 4.
Figure 21 is the single ZnO meso-porous nanos fibre section scanning electron microscope (SEM) photograph obtained by the embodiment of the present invention 4.
Scanning electron microscope (SEM) photograph under the low resolution multiplying power of solid precursor nano wires of the Figure 22 obtained by the embodiment of the present invention 5.
Figure 23 is the scanning electron microscope (SEM) photograph in the single solid precursor nano wire section obtained by the embodiment of the present invention 5.
Figure 24, which is that the ZnO meso-porous nano fibers obtained by the embodiment of the present invention 5 are low, differentiates scanning electron microscope (SEM) photograph under multiplying power.
Scanning electron microscope (SEM) photograph under ZnO meso-porous nano fiber high-resolution multiplying powers of the Figure 25 obtained by the embodiment of the present invention 5.
Figure 26 is the single ZnO meso-porous nanos fibre section scanning electron microscope (SEM) photograph obtained by the embodiment of the present invention 5.
Scanning electron microscope (SEM) photograph under the low resolution multiplying power of solid precursor nano wires of the Figure 27 obtained by comparative example 1 of the present invention.
Figure 28 is the scanning electron microscope (SEM) photograph in the single solid precursor nano wire section obtained by comparative example 1 of the present invention.
Figure 29, which is that the ZnO nano fiber obtained by comparative example 1 of the present invention is low, differentiates scanning electron microscope (SEM) photograph under multiplying power.
Scanning electron microscope (SEM) photograph under ZnO nano fiber high-resolution multiplying powers of the Figure 30 obtained by comparative example 1 of the present invention.
Figure 31 is the single ZnO nano fibre section scanning electron microscope (SEM) photograph obtained by comparative example 1 of the present invention.
Specific embodiment
It is specific embodiments of the present invention below, and is described with reference to the drawings and technical scheme work is further retouched
It states, but the present invention is not limited to these embodiments.
Embodiment 1：
1.0g PVP are dissolved in 6g ethyl alcohol, the thick liquid of stirring extremely formation homogeneous transparent under room temperature.Then add in
The TS of 2.5g ZnAc, 6g deionized waters and 0.6g, obtains mixed liquor, and in 60 DEG C of heating water baths mixed liquor was formed Huang in 30 minutes
The PVP/ZnAc/TS spinning liquid as precursor of color.
Then after the spinning liquid as precursor configured is stood in injected plastic needle tubing, and it is horizontally placed on spinning-drawing machine.Gold
Belong to syringe needle (internal diameter 0.41mm) and make electrospinning wire anode, wire netting is made to receive the cathode of material, the distance between anode and cathode
For 18cm, electrostatic spinning is carried out under 12.5kV high pressures, the presoma nano wire of high-purity is prepared.Then presoma is received
When rice noodles are placed in that drying process 9 is small in 70 DEG C of constant temperature drying boxes, solid precursor nano wire is obtained.
Finally solid precursor nano wire is placed in crucible, is heated up in air atmosphere with the heating rate of 3 DEG C/min
To 480 DEG C heat preservation 2 it is small when calcined, then furnace cooling obtains ZnO meso-porous nano fibers.
Embodiment 2：
1.0g PVP are dissolved in 6g ethyl alcohol, the thick liquid of stirring extremely formation homogeneous transparent under room temperature.Then add in
The TS of 2.5g ZnAc, 6g deionized waters and 0.5g, obtains mixed liquor, and in 60 DEG C of heating water baths mixed liquor was formed Huang in 30 minutes
The PVP/ZnAc/TS spinning liquid as precursor of color.
Then after the spinning liquid as precursor configured is stood in injected plastic needle tubing, and it is horizontally placed on spinning-drawing machine.Gold
Belong to syringe needle (internal diameter 0.41mm) and make electrospinning wire anode, wire netting is made to receive the cathode of material, the distance between anode and cathode
For 18cm, electrostatic spinning is carried out under 12.5kV high pressures, the presoma nano wire of high-purity is prepared.Then presoma is received
Rice noodles be placed in 70 DEG C of constant temperature drying box drying process 9 it is small when, obtain solid precursor nano wire.
Finally solid precursor nano wire is placed in crucible, is heated up in air atmosphere with the heating rate of 3 DEG C/min
To 480 DEG C heat preservation 2 it is small when calcined, then furnace cooling obtains ZnO meso-porous nano fibrous materials.
Embodiment 3：
1.0g PVP are dissolved in 6g ethyl alcohol, the thick liquid of stirring extremely formation homogeneous transparent under room temperature.Then add in
The TS of 2.5g ZnAc, 6g deionized waters and 0.7g, obtains mixed liquor, and in 60 DEG C of heating water baths mixed liquor was formed Huang in 30 minutes
The PVP/ZnAc/TS spinning liquid as precursor of color.
Then after the spinning liquid as precursor configured is stood in injected plastic needle tubing, and it is horizontally placed on spinning-drawing machine.Gold
Belong to syringe needle (internal diameter 0.41mm) and make electrospinning wire anode, wire netting is made to receive the cathode of material, the distance between anode and cathode
For 18cm, electrostatic spinning is carried out under 12.5kV high pressures, the presoma nano wire of high-purity is prepared.Then presoma is received
Rice noodles be placed in 70 DEG C of constant temperature drying box drying process 9 it is small when, obtain solid precursor nano wire.
Finally solid precursor nano wire is placed in crucible, is heated up in air atmosphere with the heating rate of 3 DEG C/min
To 480 DEG C heat preservation 2 it is small when calcined, then furnace cooling obtains ZnO meso-porous nano fibrous materials.
Embodiment 4：
1.0g PVP are dissolved in 6g ethyl alcohol, the thick liquid of stirring extremely formation homogeneous transparent under room temperature.Then add in
The TS of 2.5g ZnAc, 6g deionized waters and 0.25g, obtains mixed liquor, and in 60 DEG C of heating water baths mixed liquor was formed Huang in 30 minutes
The PVP/ZnAc/TS spinning liquid as precursor of color.
Then after the spinning liquid as precursor configured is stood in injected plastic needle tubing, and it is horizontally placed on spinning-drawing machine.Gold
Belong to syringe needle (internal diameter 0.41mm) and make electrospinning wire anode, wire netting is made to receive the cathode of material, the distance between anode and cathode
For 18cm, electrostatic spinning is carried out under 12.5kV high pressures, the presoma nano wire of high-purity is prepared.Then it is presoma is fine
Dimension be placed in 70 DEG C of constant temperature drying box drying process 9 it is small when, obtain solid precursor nano wire.
Finally solid precursor nano wire is placed in crucible, is heated up in air atmosphere with the heating rate of 3 DEG C/min
To 480 DEG C heat preservation 2 it is small when calcined, then furnace cooling obtains mesoporous cylindric ZnO nano fibrous material.
Embodiment 5：
1.0g PVP are dissolved in 6g ethyl alcohol, the thick liquid of stirring extremely formation homogeneous transparent under room temperature.Then add in
The TS of 2.5g ZnAc, 6g deionized waters and 0.4g, obtains mixed liquor.Mixed liquor is formed into Huang in 30 minutes in 60 DEG C of heating water baths
The PVP/ZnAc/TS spinning liquid as precursor of color.
Then after the spinning liquid as precursor configured is stood in injected plastic needle tubing, and it is horizontally placed on spinning-drawing machine.Gold
Belong to syringe needle (internal diameter 0.41mm) and make electrospinning wire anode, wire netting is made to receive the cathode of material, the distance between anode and cathode
For 18cm, electrostatic spinning is carried out under 12.5kV high pressures, the presoma nano wire of high-purity is prepared.Then presoma is received
Rice noodles be placed in 70 DEG C of constant temperature drying box drying process 9 it is small when, obtain solid precursor nano wire.
Finally solid precursor is placed in crucible, is warming up to 480 DEG C in air atmosphere with the heating rate of 3 DEG C/min
Keep the temperature 2 it is small when calcined, then furnace cooling obtains mesoporous elliptic cylindrical shape ZnO nano fibrous material.
Comparative example 1：
1.0g PVP are dissolved in 6g ethyl alcohol, the thick liquid of stirring extremely formation homogeneous transparent under room temperature.Then add in
2.5g ZnAc, 6g deionized waters, obtain mixed liquor.Mixed liquor is formed into transparent PVP/ in 30 minutes in 60 DEG C of heating water baths
ZnAc spinning liquid as precursor.
Then after the spinning liquid as precursor configured is stood in injected plastic needle tubing, and it is horizontally placed on spinning-drawing machine.Gold
Belong to syringe needle (internal diameter 0.41mm) and make electrospinning wire anode, wire netting is made to receive the cathode of material, the distance between anode and cathode
For 18cm, electrostatic spinning is carried out under 12.5kV high pressures, the presoma nano wire of high-purity is prepared.Then by precursor tape
Material be placed in 70 DEG C of constant temperature drying box drying process 9 it is small when, obtain solid precursor nano wire.
Finally solid precursor nano wire is placed in crucible, is heated up in air atmosphere with the heating rate of 3 DEG C/min
To 480 DEG C heat preservation 2 it is small when calcined, then furnace cooling obtains non-porous column ZnO nano fibrous material.
Scanning electron microscope under the low resolution multiplying power of the solid-state precursor nano wire of Fig. 1, Fig. 2 obtained by the embodiment of the present invention 1
Figure and solid-state precursor nano wire cross-sectional scans electron microscope, it is solid-state precursor nano wire to show the material being prepared.
Fig. 3, Fig. 4 are the typical low power of the high-purity ZnO meso-porous nano fibrous materials prepared by embodiment 1 and high power scanning
Electromicroscopic photograph shows the mesoporous banded structure nano material that prepared material is high-purity.
Fig. 5 is the cross-sectional scans electron microscope of the single ZnO meso-porous nanos fiber prepared by embodiment 1, further proves institute
The material being prepared is the nano material of banded structure.
Fig. 6 is the corresponding X-ray diffraction of nano material (XRD) collection of illustrative plates of the banded structure prepared by embodiment 1, is shown
Prepared meso-porous nano carrying material is six pure side's Pb-Zn deposits phases, and with good crystallinity.
Scanning electron microscope under the low resolution multiplying power of the solid-state precursor nano wire of Fig. 7, Fig. 8 obtained by the embodiment of the present invention 2
Figure and single solid-state precursor nano wire cross-sectional scans electron microscope, it is solid-state precursor nano wire to show the material being prepared.
Fig. 9, Figure 10 are the typical low power of high-purity ZnO nano-band material and high power scanning electron microscope prepared by embodiment 2
Photo shows the ZnO meso-porous nano fibrous materials that prepared material is high-purity.
Figure 11 is the cross-sectional scans photo of the single ZnO nano-band prepared by embodiment 2, is clearly indicated out prepared
The rectangular cross-section of nano material has convincingly demonstrated the ZnO nano-band that the nano material being prepared is meso-hole structure.
Figure 12, Figure 13 are to scan electricity under the low resolution multiplying power of the solid-state precursor nano wire obtained by the embodiment of the present invention 3
Mirror figure and single solid-state precursor nano wire cross-sectional scans electron microscope, it is solid-state precursor nanometer to show the material being prepared
Line.
Figure 14, Figure 15 are the typical low power of high-purity ZnO nano-band material and high power scanning electron microscope prepared by embodiment 3
Photo shows the ZnO meso-porous nano fibrous materials that prepared material is high-purity.
Figure 16 is the cross-sectional scans photo of the single ZnO nano-band prepared by embodiment 3, is clearly indicated out prepared
The rectangular cross-section of nano material has convincingly demonstrated the ZnO nano-band that the nano material being prepared is meso-hole structure.
Figure 17, Figure 18 are to scan electricity under the low resolution multiplying power of the solid-state precursor nano wire obtained by the embodiment of the present invention 4
Mirror figure and single solid-state precursor nano wire cross-sectional scans electron microscope, it is solid-state precursor nanometer to show the material being prepared
Line.
Figure 19, Figure 20 are that the typical low power of the ZnO nano fibrous material prepared by embodiment 4 and high power scanning electron microscope are shone
Piece, it is meso-hole structure ZnO nano fibrous material to show prepared material.
Figure 21 is the cross-sectional scans photo of the single ZnO nano fiber prepared by embodiment 4, is clearly indicated out prepared
The section of nano material be circle, it was demonstrated that the material being prepared is mesoporous cylindrical nanofibers.
Figure 22, Figure 23 are to scan electricity under the low resolution multiplying power of the solid-state precursor nano wire obtained by the embodiment of the present invention 5
Mirror figure and single solid-state precursor nano wire cross-sectional scans electron microscope, it is solid-state precursor nanometer to show the material being prepared
Line.
Figure 24, Figure 25 are that the typical low power of the ZnO nano fibrous material prepared by embodiment 5 and high power scanning electron microscope are shone
Piece shows the ZnO meso-porous nano fibrous materials that prepared material is high-purity.
Figure 26 is the cross-sectional scans photo of the single ZnO nano fiber prepared by embodiment 5, is clearly indicated out prepared
The section of nano material be ellipse, it is elliptic cylindrical shape ZnO meso-porous nanos to have convincingly demonstrated the nano material that is prepared
Fiber.
Figure 27, Figure 28 are to scan electricity under the low resolution multiplying power of the solid-state precursor nano wire obtained by comparative example 1 of the present invention
Mirror figure and single solid-state precursor nano wire cross-sectional scans electron microscope, it is solid-state precursor nanometer to show the material being prepared
Line.
Figure 29, Figure 30 are the typical low power of the high-purity ZnO nano fibrous material prepared by comparative example 1 and high power scanning electricity
Mirror photo shows the non-porous ZnO nano fibrous material that prepared material is high-purity.
Figure 31 is the cross-sectional scans picture of the single ZnO nano fiber prepared by comparative example 1, is clearly indicated out prepared
The section of nano material be circle, it is non-porous cylindrical nanofibers to have convincingly demonstrated the material that is prepared.
In above-described embodiment and its alternative, when PVP/ZnAc/TS spinning liquid as precursor configures, the dosage of ethyl alcohol may be used also
Think 3g, 4g, 5g, 7g, 8g, 9g.
In above-described embodiment and its alternative, when PVP/ZnAc/TS spinning liquid as precursor configures, the dosage of ZnAc may be used also
Think 2g, 3g, 4g, 5g.
In above-described embodiment and its alternative, when PVP/ZnAc/TS spinning liquid as precursor configures, the dosage of TS can be with
For 0.01g, 0.05g, 0.1g, 0.15g, 0.2g, 0.3g, 0.35g, 0.45g, 0.55g, 0.65g, 0.75g, 0.8g, 0.85g,
0.9g、0.95g、1g。
In above-described embodiment and its alternative, during electrostatic spinning, the spacing of anode and cathode can also be 19cm,
19.5cm、20.5cm、21cm、21.5cm、22cm、22.5cm、23cm、23.5cm、23.5cm、24cm、24.5cm、25cm.It is quiet
The voltage of Electrospun can also be 12kV, 12.1kV, 12.2kV, 12.3kV, 12.4kV, 12.6kV, 12.7kV, 12.8kV,
12.9kV、13kV。
In above-described embodiment and its alternative, during electrostatic spinning, presoma nano wire is placed in constant temperature drying box
Drying temperature can also be 50 DEG C, 52 DEG C, 56 DEG C, 58 DEG C, 60 DEG C, 63 DEG C, 66 DEG C, 69 DEG C, 71 DEG C, 73 DEG C, 76 DEG C, 77 DEG C,
78℃、80℃.Drying time can also be 8h, 8.2h, 9.6h, 8.8h, 10.3h, 10.6h, 11.9h, 12.1h, 12.3h,
12.6h、13.7h、13.4h、14h。
In above-described embodiment and its alternative, during electrostatic spinning, precursor nano wire room temperature can also be dried in the shade, room temperature
Time of aeration-drying at ambient temperature of drying in the shade can be 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h, for 24 hours, wind of divulging information
Speed can be 1m/s, 1.3m/s, 1.5m/s, 1.6m/s, 1.8m/s, 2m/s.
In above-described embodiment and its alternative, when precursor nano wire is through high-temperature calcination, calcining heat can also be 392
℃、300℃、310℃、320℃、330℃、340℃、350℃、360℃、370℃、377℃、478℃.Calcination time can be with
For 1h, 1.2h, 1.6h, 1.8h, 1.4h, 2.6h, 2.9h, 2.1h, 2.3h, 2.6h, 2.7h, 2.4h, 3h.Heating rate can be with
For 2 DEG C/min, 2.5 DEG C/min, 2.8 DEG C/min, 3.5 DEG C/min, 3.8 DEG C/min, 4 DEG C/min.
In above-described embodiment and its alternative, when precursor nano wire is through high-temperature calcination, calcination environment can also be hydrogen
Atmosphere either carbon monoxide atmosphere or oxygen atmosphere or other atmosphere of inert gases including helium, nitrogen.
In view of the present invention program embodiment is numerous, each embodiment experimental data is huge numerous, is not suitable for arranging one by one herein
Explanation is lifted, but the content verified required for each embodiment and obtained final conclusion are close, so herein not to each reality
The verification content for applying example is illustrated one by one, only illustrates the excellent part of the present patent application using embodiment 1-5 as representative.
It, equally all will in the present invention in place of this place embodiment is to the claimed non-limit of technical scope midrange
In the range of asking protection.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology belonging to the present invention is led
The technical staff in domain can do various modifications or supplement to described specific embodiment or substitute in a similar way, but simultaneously
The spirit or beyond the scope of the appended claims of the present invention is not deviated by.
It is skilled to this field although having been made a detailed description to the present invention and being cited some specific embodiments
For technical staff, as long as it is obvious that can make various changes or correct without departing from the spirit and scope of the present invention.
Claims (7)
1. a kind of preparation method of ZnO meso-porous nanos fiber, it is characterised in that：The preparation method is：Appropriate PVP is dissolved in second
In alcohol, stirring at normal temperature obtains transparent and homogeneous solution, then adds in zinc acetate, water and TS, then heating water bath obtains yellow PVP/
ZnAc/TS spinning liquid as precursor, by prepared spinning liquid as precursor after spinning obtains precursor nano wire, through high-temperature calcination
Obtain ZnO meso-porous nano fibers.
2. the preparation method of ZnO meso-porous nanos fiber according to claim 1, it is characterised in that：The PVP/ZnAc/TS
Spinning liquid as precursor obtains precursor nano wire through electrostatic spinning, and the wherein voltage of electrostatic spinning is 12-13kV, cathode and anode
The distance between be 18-25cm.
3. the preparation method of ZnO meso-porous nanos fiber according to claim 1, it is characterised in that：The PVP/ZnAc/TS
The mass ratio of ethyl alcohol and water is (3-1) when spinning liquid as precursor configures：1, wherein water is deionized water or distilled water.
4. the preparation method of ZnO meso-porous nanos fiber according to claim 1, it is characterised in that：The PVP/ZnAc/TS
It is dissolved in when spinning liquid as precursor configures per 1gPVP in 3-9g ethyl alcohol.
5. the preparation method of ZnO meso-porous nanos fiber according to claim 1, it is characterised in that：The PVP/ZnAc/TS
Spinning liquid as precursor configure when spinning solution in often containing 1gPVP then ZnAc usage amount be 2-5g.
6. the preparation method of ZnO meso-porous nanos fiber according to claim 1, it is characterised in that：The PVP/ZnAc/TS
Often containing 1gPVP, then TS usage amounts are 0.01-1g in spinning solution when spinning liquid as precursor configures.
7. the preparation method of ZnO meso-porous nanos fiber according to claim 1, it is characterised in that：The high-temperature calcination is
The heat preservation calcining 1-3h at 300-480 DEG C of calcining heat, heating rate is 2-4 DEG C/min during calcining.
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| CN201510386289.XA CN105002598B (en) | 2015-07-01 | 2015-07-01 | A kind of preparation method of ZnO meso-porous nanos fiber |
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