CN108956710A - A kind of preparation method of the spiral porous hollow nanowire sensor of latticed ZnO - Google Patents
A kind of preparation method of the spiral porous hollow nanowire sensor of latticed ZnO Download PDFInfo
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- CN108956710A CN108956710A CN201810558838.0A CN201810558838A CN108956710A CN 108956710 A CN108956710 A CN 108956710A CN 201810558838 A CN201810558838 A CN 201810558838A CN 108956710 A CN108956710 A CN 108956710A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses a kind of preparation methods of latticed spiral porous hollow nanowire sensor of ZnO, this method is using spinning solution as raw material, first presoma is prepared using electrostatic spinning on ITO electro-conductive glass, presoma is transferred to calcining in resistance furnace again and obtains the latticed spiral porous hollow nano wire of ZnO, then in the spiral porous hollow nano wire surrounding coating Ag Au electrode of latticed ZnO or conducting resinl, and extraction wire, it can be obtained the gas sensor of structure completion, this method controllability is good, simple process, transducer sensitivity that is at low cost and obtaining is high.
Description
Technical field
The invention belongs to sensor preparation technical fields, relate generally to a kind of spiral porous hollow nanometer of latticed ZnO
The preparation method of line sensor.
Background technique
Sensor is a very important field in current scientific development, it can be in smart home, safety in production, ring
The fields such as border protection, national defence play positive effect.Therefore, high-performance sensors are always the target that scientific research personnel makes great efforts.Si
Have many advantages, such as that mature preparation process, low in cost, size is big, thus Si based sensor gets more and more people's extensive concerning.In order to
Realizing Si based sensor, people perform etching generally by high quality Si substrate, Si nano-array is obtained on a si substrate,
Then increase Au electrode and draw Au line, to constitute complete sensor structure.
However, the minimum detection limit of Si nano-array sensor is generally 100ppm, it is far second to other semiconductor sensings
Device (5-10ppm).In addition, its corresponding time is generally 30-50s, i.e. its sensitivity is also required to further increase.In addition to Si
Based sensor, zno-based sensor are also subject to the people's attention.ZnO have it is electrical and optical have excellent performance, be nontoxic, raw material
Abundant, the advantages that preparation process is relatively easy, thus, it is widely used in field of semiconductor devices.
Currently, Au/ZnO nano column array sensor minimum detection limit is generally 10ppm, it is better than Si nano-array biography
Sensor.However, the shortcomings that prior art, has:
1.ZnO nano-pillar/nano wire preparation process is more complex, higher cost；
2. vertical distribution ZnO nano column/nano wire electric signal propagation path is longer, the sensor response time is longer.
Summary of the invention
The purpose of the present invention is be to provide a kind of spiral porous air of latticed ZnO in order to overcome the deficiencies of the prior art
The preparation method of heart nanowire sensor can improve the production technology of ZnO nano-wire using method of the invention, reduce technique
Complexity and production cost and improve sensor response sensitivity.
The technical solution adopted by the present invention is that: a kind of preparation of the latticed spiral porous hollow nanowire sensor of ZnO
Method, comprising the following steps:
A. the preparation of precursor fibre:
Inorganic matter/PVP spinning solution is prepared, electrostatic spinning is carried out, it is fine that latticed spiral inorganic matter/PVP presoma is made
Dimension；The inorganic matter/PVP spinning solution is Zn (NO3)2·4H2O、Zn(CH2COO)2·4H2O、Al(NO3)3·6H2O's and PVP
Mixed solution；
B. the preparation of nano wire:
By latticed spiral inorganic matter/PVP precursor fibre calcining, it is spirally porous to obtain latticed Al doping ZnO
Hollow Nano line；
C. the preparation of sensor:
Conductive electrode, and extraction wire are coated in the spiral porous hollow nano wire surrounding of latticed Al doping ZnO, can be obtained
Obtain the latticed spiral porous hollow nanowire sensor of ZnO.
Preferably, the inorganic matter/PVP spinning solution preparation method is: by Zn (NO3)2·4H2O、Zn(CH2COO)2·
4H2O and Al (NO3)3·6H2O mixing, obtains inorganic matter；Inorganic matter is dissolved in deionized water, poly- second PVP is added, stirs 30-
90min stands, obtains inorganic matter/PVP spinning solution.
Preferably, Zn (NO3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·6H2The mass ratio of O is 1:0.5-
3:0.01-0.05。
Preferably, in the inorganic matter/PVP spinning solution, the concentration of PVP is 40-50wt%, mineral concentration 8-
15wt%.It is furthermore preferred that the concentration of PVP is 46wt%, mineral concentration 10wt%.
Preferably, the molecular weight of PVP is 2000-50000.
Preferably, the grid of the latticed spiral inorganic matter/PVP precursor fibre is square, its side length is
400-2500nm。
Preferably, in step B, the condition of calcination process control are as follows: 1-5 DEG C of heating rate/min is warming up to 600-900
DEG C, it calcines 8-16 hours.
Preferably, the electrode is Ag electrode, Au electrode or conducting resinl.
Preferably, the sensor is gas sensor.
More specifically, specific step is as follows for the preparation method of the spiral porous hollow nanowire sensor of latticed ZnO:
(1) Zn (NO for being 1:0.5-3:0.015 by mass ratio3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·
6H2O, uniformly mixing, is dissolved in deionized water, weighs a certain amount of molecular weight polyethylene pyrrolidones (PVP (K40)), at room temperature
30-120min is stirred, standing can be obtained spinning solution, and the content of the PVP in spinning solution is 46wt%, and inorganic salt content is
10wt%；
(2) on ITO electro-conductive glass, using electrostatic spinning, latticed spiral inorganic matter/PVP precursor fibre is prepared,
Grid is square, side length 400-2500nm；
(3) precursor fibre is transferred in chamber type electric resistance furnace, the heating rate of then 1-5 DEG C/min is warming up to 600-
It 900 DEG C, calcines 8-16 hours, can be obtained the spiral porous hollow nano wire of latticed ZnO；
(4) in the spiral porous hollow nano wire surrounding coating Ag Au electrode of latticed ZnO or conducting resinl, and draw
Conducting wire out can be obtained the gas sensor of structure completion.
Beneficial effects of the present invention are as follows: (1) preparing ZnO nano-wire using electrostatic spinning, controllability is good, and is conducive to drop
Low complex process degree and production cost；(2) ZnO nano-wire is changed to plane formula distribution, shortens the propagation distance of signal, favorably
In the sensitivity for improving response device.
Detailed description of the invention
Fig. 1 is the schematic diagram of the latticed Al doping porous spiral-type nanometer line gas sensor of ZnO, wherein 11 be ITO lining
Bottom, 12 be the latticed Al doping porous spiral-type nanometer line of ZnO, and 13 be electrode.
Specific embodiment
In order to preferably explain the present invention, it is described further now in conjunction with following specific embodiments, but the present invention is unlimited
In specific embodiment.
Embodiment 1
Zn (the NO for being 1:0.5:0.01 by mass ratio3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·6H2O、
Uniformly mixing, is dissolved in deionized water, weighs the polyvinylpyrrolidone (PVP (K40)) that a certain amount of molecular weight is 2000, room temperature
Lower stirring 30min, standing can be obtained spinning solution, and wherein the concentration of the PVP in spinning solution is 40wt%, and inorganic salt concentration is
10wt%；
Latticed spiral inorganic matter/PVP precursor fibre, grid are prepared using electrostatic spinning on ITO electro-conductive glass
It is square, side length 1000nm；
Precursor fibre is transferred in chamber type electric resistance furnace, then the heating rate of 1 DEG C/min, is warming up to 600 DEG C, calcining
8 hours, it can be obtained the spiral porous hollow nano wire of latticed ZnO；
Au electrode, and extraction wire are led in the spiral porous hollow nano wire surrounding coating of latticed ZnO, can be obtained gas
Dependent sensor.
The structure of resulting gas sensor is as shown in Figure 1.
Embodiment 2
Zn (the NO for being 1:1:0.015 by mass ratio3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·6H2O,
Even mixing, is dissolved in deionized water, weighs the polyvinylpyrrolidone (PVP (K40)) that a certain amount of molecular weight is 30000, room temperature
Lower stirring 60min, standing can be obtained spinning solution, and wherein the concentration of the PVP in spinning solution is 45wt%, and inorganic salt concentration is
10wt%；
Latticed spiral inorganic matter/PVP precursor fibre, grid are prepared using electrostatic spinning on ITO electro-conductive glass
It is square, side length 1000nm；
Precursor fibre is transferred in chamber type electric resistance furnace, then the heating rate of 1 DEG C/min, is warming up to 600 DEG C, calcining
8 hours, it can be obtained the spiral porous hollow nano wire of latticed ZnO；
Au electrode, and extraction wire are led in the spiral porous hollow nano wire surrounding coating of latticed ZnO, can be obtained gas
Dependent sensor.
Embodiment 3
Zn (the NO for being 1:2:0.02 by mass ratio3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·6H2O,
Even mixing, is dissolved in deionized water, weighs the polyvinylpyrrolidone (PVP (K40)) that a certain amount of molecular weight is 50000, room temperature
Lower stirring 90min, standing can be obtained spinning solution, and wherein the concentration of the PVP in spinning solution is 50wt%, and inorganic salt concentration is
10wt%；
Latticed spiral inorganic matter/PVP precursor fibre, grid are prepared using electrostatic spinning on ITO electro-conductive glass
It is square, side length 1000nm；
Precursor fibre is transferred in chamber type electric resistance furnace, then the heating rate of 1 DEG C/min, is warming up to 600 DEG C, calcining
8 hours, it can be obtained the spiral porous hollow nano wire of latticed ZnO；
Au electrode, and extraction wire are led in the spiral porous hollow nano wire surrounding coating of latticed ZnO, can be obtained gas
Dependent sensor.
Embodiment 4
Zn (the NO for being 1:2.5:0.03 by mass ratio3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·6H2O、
Uniformly mixing, is dissolved in deionized water, weighs the polyvinylpyrrolidone (PVP (K40)) that a certain amount of molecular weight is 30000, room
Temperature is lower to stir 60min, and standing can be obtained spinning solution, and wherein the concentration of the PVP in spinning solution is 45wt%, and inorganic salt concentration is
10wt%；
Latticed spiral inorganic matter/PVP precursor fibre, grid are prepared using electrostatic spinning on ITO electro-conductive glass
It is square, side length 1000nm；
Precursor fibre is transferred in chamber type electric resistance furnace, then the heating rate of 3 DEG C/min, is warming up to 750 DEG C, calcining
12 hours, it can be obtained the spiral porous hollow nano wire of latticed ZnO；
Au electrode, and extraction wire are led in the spiral porous hollow nano wire surrounding coating of latticed ZnO, can be obtained gas
Dependent sensor.
Embodiment 5
Zn (the NO for being 1:3:0.05 by mass ratio3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·6H2O,
Even mixing, is dissolved in deionized water, weighs the polyvinylpyrrolidone (PVP (K40)) that a certain amount of molecular weight is 3, stirs at room temperature
60min is mixed, standing can be obtained spinning solution, and wherein the concentration of the PVP in spinning solution is 45wt%, and inorganic salt concentration is
10wt%；
Latticed spiral inorganic matter/PVP precursor fibre, grid are prepared using electrostatic spinning on ITO electro-conductive glass
It is square, side length 1000nm；
Precursor fibre is transferred in chamber type electric resistance furnace, then the heating rate of 5 DEG C/min, is warming up to 900 DEG C, calcining
16 hours, it can be obtained the spiral porous hollow nano wire of latticed ZnO；
Au electrode is led in the spiral porous hollow nano wire surrounding coating of latticed ZnO, extraction wire can gas sensing
Device.
Claims (9)
1. a kind of preparation method of the spiral porous hollow nanowire sensor of latticed ZnO, which is characterized in that including following step
It is rapid:
A. the preparation of precursor fibre:
Inorganic matter/PVP spinning solution is prepared, electrostatic spinning is carried out, latticed spiral inorganic matter/PVP precursor fibre is made；Institute
Stating inorganic matter/PVP spinning solution is Zn (NO3)2·4H2O、Zn(CH2COO)2·4H2O、Al(NO3)3·6H2The mixing of O and PVP is molten
Liquid；
B. the preparation of nano wire:
By latticed spiral inorganic matter/PVP precursor fibre calcining, the latticed Al doping spiral porous hollow of ZnO is obtained
Nano wire；
C. the preparation of sensor:
Conductive electrode, and extraction wire are coated in the spiral porous hollow nano wire surrounding of latticed Al doping ZnO, can be obtained net
The spiral porous hollow nanowire sensor of trellis ZnO.
2. preparation method according to claim 1, which is characterized in that the inorganic matter/PVP spinning solution preparation method
It is: by Zn (NO3)2·4H2O、Zn(CH2COO)2·4H2O and Al (NO3)3·6H2O mixing, obtains inorganic matter；Inorganic matter is molten
In deionized water, PVP is added, stirs 30-90min, stands, obtains inorganic matter/PVP spinning solution.
3. preparation method according to claim 2, which is characterized in that Zn (NO3)2·4H2O、Zn(CH2COO)2·4H2O and
Al(NO3)3·6H2The mass ratio of O is 1:0.5-3:0.01-0.05.
4. preparation method according to claim 2, which is characterized in that in the inorganic matter/PVP spinning solution, the concentration of PVP
For 40-50wt%, mineral concentration 8-15wt%.
5. preparation method according to claim 2, which is characterized in that the molecular weight of PVP is 2000-50000.
6. preparation method according to claim 1, which is characterized in that the latticed spiral inorganic matter/PVP presoma
The grid of fiber is square, and its side length is 400-2500nm.
7. preparation method according to claim 1, which is characterized in that in step B, the condition of calcination process control are as follows: rise
1-5 DEG C of warm rate/min is warming up to 600-900 DEG C, calcines 8-16 hours.
8. preparation method according to claim 1, which is characterized in that the electrode is Ag electrode, Au electrode or conduction
Glue.
9. preparation method according to claim 1, which is characterized in that the sensor is gas sensor.
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