CN108918630A - A kind of preparation method of Al doping ZnO ultrathin nanometer piece sensitive material and the purposes of gained nano sensitive material - Google Patents
A kind of preparation method of Al doping ZnO ultrathin nanometer piece sensitive material and the purposes of gained nano sensitive material Download PDFInfo
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- CN108918630A CN108918630A CN201810466967.7A CN201810466967A CN108918630A CN 108918630 A CN108918630 A CN 108918630A CN 201810466967 A CN201810466967 A CN 201810466967A CN 108918630 A CN108918630 A CN 108918630A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
A kind of preparation method of Al doping ZnO ultrathin nanometer piece sensitive material and the purposes of gained nano sensitive material, which is by Al2O3After the effective ultrapure water of ceramics, ethyl alcohol, acetone, ultrapure water are successively cleaned by ultrasonic, Al nanometers of middle layers are grown on its surface using direct current magnetron sputtering process, the ceramic tube for growing Al nanometers of middle layers is put into zinc acetate methanol solution ultrasonic, it places it in Muffle furnace and heats again, be cooled to room temperature growth ZnO seed layer；The ceramic tube of digestion solution and growth seed layer is put into autoclave, then after reaction kettle is placed in a vacuum drying oven hydro-thermal process, places into Muffle furnace and anneals, obtains that the ultra-thin ZnO nano piece of Al doping can be grown in ceramic pipe surface.This method preparation process is simple, process cleans are pollution-free and cost is relatively low, and gained ultrathin nanometer piece, which prepares gas sensor as sensitive material, can realize detection to alcohol gas.
Description
Technical field
The invention belongs to gas detection technology fields, and in particular to a kind of Al doping ZnO for alcohol gas sensor
The preparation method of ultrathin nanometer piece sensitive material.
Background technique
Gas sensor has a wide range of applications in numerous areas such as environmental monitoring, biomedicine, military and national defenses.Air-sensitive material
Material is the important of decision gas sensor performance (such as response, detection limit, response-recovery time, stability and anti-interference)
Factor, metal-oxide semiconductor (MOS) are concerned as novel gas sensitive, and the absorption of surface gas and desorption can cause
The transformation of resistance.ZnO is one of common Metal oxide semiconductor gas-sensitiveness material, is had in the application aspect of gas sensor
Many advantages have very high sensitivity, and rich content, cheap, nothing to many oxidisability or reducibility gas
Poison is pollution-free, it is simple etc. to prepare.The ZnO material of nanoscale has big specific surface area, and surface exposure atomicity is more, because
This has more excellent gas-sensitive property.Up to the present, the ZnO nano material of different size and shapes is successfully prepared
Come.The disadvantages of existing generally existing operating temperature of gas sensor is higher, the response-recovery time is longer, detection limit is higher,
And two-dimentional ZnO nano-structure usually has more surface defects and surface energy, is extremely suitable for as gas sensitive；Especially
When the thickness of two-dimentional ZnO nano-structure is close or is less than Debye length, which has superior gas-sensitive property.
On the other hand, electronic state structure can be changed by carrying out element doping to ZnO, so as to improve its air-sensitive performance.Therefore, it researches and develops
A kind of novel gas sensor material of the ZnO of two-dimensional nanostructure is significantly.
Summary of the invention
It is sensitive to provide a kind of Al doping ZnO ultrathin nanometer piece for defect existing for existing gas sensor by the present invention
The preparation method of material, and be used for alcohol gas sensor, obtained sensor to alcohol gas have high response,
Low detectable limit, fast response and resume speed, while it is with good stability with it is selective.
Technical solution of the present invention
A kind of preparation method of the Al doping ZnO ultrathin nanometer piece sensitive material for alcohol gas sensor specifically includes
Following steps：
Step 1, by Al2O3The effective ultrapure water of ceramics, ethyl alcohol, acetone, ultrapure water are successively cleaned by ultrasonic 5-10min, then
With being dried with nitrogen；
Step 2, the ceramic tube that will be cleaned grow Al nanometers of middle layers on its surface using direct current magnetron sputtering process, splash
Penetrating technological parameter is：The purity of Al target is 99.99%, and background vacuum is not less than 1 × 10-4Pa, sputtering power 100-
150W, argon flow 15-30sccm, sputtering pressure 0.5-1Pa, target-substrate distance 5-8cm, substrate do not heat, pre-sputtering 10-
20min, when sputtering a length of 30-60s；
Step 3 configures zinc acetate methanol solution, is at room temperature dispersed in the zinc acetate of 0.55g by magnetic agitation 2h
In methanol, the concentration for obtaining zinc acetate methanol solution is 0.5mol/L；The ceramic tube for growing Al nanometers of middle layers is put into acetic acid
Ultrasound 5-10min in zinc methanol solution, then place it in temperature and be set as heating 1h in 200 DEG C of Muffle furnace, it is cooled to room temperature,
Grow ZnO seed layer；
Step 4, configuration 0.05mol/L zinc nitrate, 0.05mol/L hexamethylenetetramine, 0.05mol/L ammonium hydroxide and
The mixed solution of 0.002mol/L polyethyleneimine, with ultrapure water it is fixed it is molten after, i.e. ZnO digestion solution；By digestion solution and growth seed
The ceramic tube of layer is put into autoclave, then reaction kettle is placed in a vacuum drying oven, and temperature is set as 100 DEG C, hydro-thermal process
After 12h, it is cooled to room temperature taking-up, by hydro-thermal method treated the effective ultrapure water of ceramics, temperature is placed into and is set as 450-
Anneal 1h in 500 DEG C of Muffle furnace.At this point, the ultra-thin ZnO nano piece of Al doping, nanometer sheet ruler can be grown in ceramic pipe surface
Very little is 1 μm -3 μm, with a thickness of 10nm-30nm.
Gas sensor is prepared using the ZnO ultrathin nanometer piece of Al doping as sensitive material, gas sensor includes ceramic tube, pottery
Sensitive layer, test electrode and heating electrode composition on porcelain tube；At a temperature of aging 1- by the gas sensor at 240-340 DEG C again
2 days, the detection to alcohol gas can be achieved by the variation of control ZnO nano material resistance；Its response to 100ppm ethyl alcohol
Value is 90, and the response-recovery time is respectively less than 2s, and detection is limited to 2ppm, and with good stability and selective.
The Al doping ultra-thin ZnO nano piece sensitive material preparation process it is simple, process cleans are pollution-free and cost compared with
Thickness low, that the Al doping zinc oxide nanometer sheet of preparation has nanoscale ultra-thin, and there are many pittings on ZnO nano piece surface.Therefore,
The ZnO nano piece has big specific surface area, more gas molecules can be adsorbed, to improve response and response-recovery
Speed；Meanwhile the doping of Al element, further improve its response and detection limit.
Detailed description of the invention
Fig. 1 (a) and (b) are respectively scanning electron microscope (SEM) figure and X that ZnO ultrathin nanometer laminated structure is grown on ceramic tube
X ray diffraction (XRD) map, Fig. 1 (c-f) are power spectrum (EDS) figure of ZnO ultrathin nanometer laminated structure, are reflected first in nanometer sheet
The distribution of element.
Fig. 2 (a) is Testing system of gas-sensor built schematic diagram；Fig. 2 (b) is at 370 DEG C of optimum working temperature, and ZnO is ultra-thin
Response-recovery curve of the nano lamellar material gas sensor to 2-600ppm ethyl alcohol；Fig. 2 (c) is optimum working temperature 370
DEG C, under conditions of concentration of alcohol is 100ppm, the stability of gas sensor and repeatability figure；Fig. 2 (d) is the sensor to not
With the response of gas.
Specific embodiment
Combined with specific embodiments below to further detailed description of the invention.The present embodiment is with technology of the invention
Implemented under premised on scheme, give detailed embodiment and specific operating process, but the present invention be not limited to
Lower embodiment.
Embodiment 1
A kind of preparation process of the Al doping ZnO ultrathin nanometer piece sensitive material for alcohol gas sensor is as follows：
The preparation of Al nanometers of middle layers is grown on ceramic tube：Ceramic tube is put into beaker first, successively using ultrapure
Water, ethyl alcohol, acetone, ultrapure water carry out ultrasonic cleaning 10min.Then use purity for 99.99% metal Al target, background is true
Reciprocal of duty cycle is 1 × 10-4Pa, sputtering power 100W, argon flow 15sccm, sputtering pressure 1Pa, target-substrate distance 8cm,
Substrate does not heat, pre-sputtering 20min, when sputtering a length of 30s, obtain the ceramic tube that surface grows Al nanometers of middle layers.
Then the ceramic tube of Al nanometers of middle layers is put into beaker growth, the zinc acetate methanol for pouring into 0.5mol/L is molten
Liquid is cleaned by ultrasonic 10min, then puts ceramic tube into crucible, is placed in temperature and is set as growing seed 1h in 200 DEG C of Muffle furnaces；It is cold
But it is placed into autoclave afterwards, pours into 1/2 digestion solution, be placed in temperature and be set as in 100 DEG C of vacuum oven, water
It is heat-treated 12h；It is cleaned repeatedly after cooling with ultrapure water, then ceramic tube is put into temperature and is set as annealing in 450 DEG C of Muffle furnace
1h takes out after it is cooled to room temperature.
Zinc acetate methanol solution therein is that the zinc acetate of 0.55g is dispersed in first by magnetic agitation 2h at room temperature
It is made in alcohol, the concentration of obtained zinc acetate methanol solution is 0.5mol/L.Digestion solution be by 0.05mol/L zinc nitrate,
0.05mol/L hexamethylenetetramine, 0.05mol/L ammonium hydroxide and 0.002mol/L polyethyleneimine configure mixed solution, and use is ultrapure
Water it is fixed it is molten after, that is, obtain ZnO digestion solution.
A piece nichrome wire is inserted into the hollow ceramic pipe, and electrode and test electrode welding will be heated at one six
On the pedestal of angle；Again by the gas sensor 340 DEG C at a temperature of aging 1 day, obtained the second of ZnO ultrathin nanometer laminated structure
Alcohol gas sensor.After completing above-mentioned steps, air-sensitive performance research can be carried out to it, as response-recovery characteristic, sensitivity are special
Property, the corresponding test such as minimum concentration, stability.
Fig. 1 (a) and (b) are respectively the SEM figure and XRD diagram that ZnO ultrathin nanometer laminated structure is grown on ceramic tube.Pass through sight
Examining SEM figure can be clearly seen that fine and close nano-sheet substance is evenly distributed in ceramic pipe surface；XRD diagram show in addition to
Al2O3The diffraction maximum of ceramic tube, other diffraction maximums belong to hexagonal wurtzite structure ZnO, any impurity diffraction maximum do not occur.Fig. 1
(c-f) it can be seen that three kinds of elements (Zn, O, Al) are evenly distributed on ZnO nano on piece, this shows that Al has successfully been doped into ZnO and has received
In rice piece.
Fig. 2 (a) is Testing system of gas-sensor built schematic diagram.Wherein RLIt is load resistance, is datum；RSIt is gas sensing
Device resistance, its value can be expressed as RS=RL(Vc-Vout)/Vout；VcIt is loop voltage, controls in 5 ± 0.1V；VoutIt is to measure
Output voltage.The system is by load resistance RLIt connects with gas sensor, by the heating voltage V for changing gas sensorh,
Make the operating temperature and the concatenated load resistance R of element of elementLOn voltage VoutIt changes, to reach testing element gas
The purpose of quick performance.
Fig. 2 (b) is at 370 DEG C of optimum working temperature, and the gas sensor of ZnO ultrathin nanometer flaky material is to different dense
Spend the response-recovery curve of ethyl alcohol (2-600ppm).ZnO nano piece gas sensor to response time of different concentration ethanol and
Recovery time is respectively less than 2s, complies fully with the technical indicator of commercial metal oxide semiconductor gas sensor.
Fig. 2 (c) is in one month under conditions of 370 DEG C of optimum working temperature, concentration of alcohol are 100ppm, every 5 days
An air-sensitive test is carried out to it.Test result is shown：The response of ZnO nano piece gas sensor is almost constant, is shown
Sensor possesses excellent stability；Fig. 2 (c) cut line sensor has preferable repeatability.
It is special to the selective gas of seven kinds of gas that Fig. 2 (d) describes the ZnO ultrathin nanometer piece gas sensor at 370 DEG C
Property, wherein various gas concentrations are 100ppm.As can be seen from the figure ZnO ultrathin nanometer piece gas sensor shows ethyl alcohol
Highest response out shows low-down response to hydrogen and carbon dioxide, to ammonia, nitrogen and methane almost without
Reaction.
Embodiment 2
A kind of preparation process of the Al doping ZnO ultrathin nanometer piece sensitive material for alcohol gas sensor is as follows：
The preparation of Al nanometers of middle layers is grown on ceramic tube：Ceramic tube is put into beaker successively using ultrapure first
Water, ethyl alcohol, acetone, ultrapure water carry out ultrasonic cleaning 5min.Then use purity for 99.99% metal Al target, background is true
Reciprocal of duty cycle is 1 × 10-4Pa, sputtering power 150W, argon flow 30sccm, sputtering pressure 0.5Pa, target-substrate distance are
6cm, substrate do not heat, pre-sputtering 15min, when sputtering a length of 1min, obtain the ceramic tube that surface grows Al nanometers of middle layers.
Then the ceramic tube of Al nanometers of middle layers is put into beaker growth, the zinc acetate methanol for pouring into 0.5mol/L is molten
Liquid is cleaned by ultrasonic 5min, then ceramic tube is put into crucible, is placed in temperature and is set as long seed 1h in 200 DEG C of Muffle furnaces；It is cooling
After be placed into autoclave, pour into 2/3 digestion solution, be placed in temperature and be set as hydro-thermal in 100 DEG C of vacuum oven
Handle 12h；It is cleaned repeatedly after cooling with ultrapure water, then ceramic tube is put into temperature and is set as the 1h that anneals in 500 DEG C of Muffle furnace,
It is taken out after it is cooled to room temperature.The configuration mode of zinc acetate methanol solution and digestion solution therein is same as Example 1.
A piece nichrome wire is inserted into the hollow ceramic pipe, and electrode and test electrode welding will be heated at one six
On the pedestal of angle, then by the gas sensor 300 DEG C at a temperature of aging 2 days, obtained the ethyl alcohol of ZnO ultrathin nanometer chip architecture
Gas sensor.
Embodiment 2 grows the ultra-thin ZnO nano piece characterization (SEM, XRD, XPS) of Al doping in ceramic pipe surface and is made
ZnO ultrathin nanometer laminated structure alcohol gas sensor gas sensitive detection effect it is similar with embodiment 1.
The preferable specific embodiment of the present invention is described in detail above.It should be appreciated that those skilled in the art without
It needs creative work according to the present invention can conceive and makes many modifications and variations.Therefore, all according to think of of the invention
In prior art basis, the scheme obtained by logic analysis or reasoning all should protect model determined by claims on road
In enclosing.
Claims (7)
1. a kind of preparation method of Al doping ZnO ultrathin nanometer piece sensitive material, it is characterized in that including following steps：
Step 1, by Al2O3The effective ultrapure water of ceramics, ethyl alcohol, acetone, ultrapure water are successively cleaned by ultrasonic 5-10min, then use nitrogen
Air-blowing is dry；
Step 2, the ceramic tube that will be cleaned grow Al nanometers of middle layers on its surface using direct current magnetron sputtering process, sputter work
Skill parameter is：The purity of Al target is 99.99%, and background vacuum is not less than 1 × 10-4Pa, sputtering power 100-150W, argon
Throughput is 15-30sccm, sputtering pressure 0.5-1Pa, target-substrate distance 5-8cm, and substrate does not heat, pre-sputtering 10-20min,
A length of 30-60s when sputtering；
The ceramic tube for growing Al nanometers of middle layers is put into ultrasound 5-10min in zinc acetate methanol solution, then is set by step 3
1h is heated in the Muffle furnace that temperature is set as 200 DEG C, is cooled to room temperature, is i.e. growth ZnO seed layer；
The ceramic tube of digestion solution and growth seed layer is put into autoclave, then reaction kettle is placed in vacuum drying by step 4
In case, temperature is set as 100 DEG C, after hydro-thermal process 12h, is cooled to room temperature taking-up, and by hydro-thermal method, treated that ceramics are effective super
Pure water rinsing places into temperature and is set as the 1h that anneals in 450-500 DEG C of Muffle furnace, at this point, can grow in ceramic pipe surface
The ultra-thin ZnO nano piece of Al doping.
2. the preparation method of Al doping ZnO ultrathin nanometer piece sensitive material according to claim 1, it is characterized in that：Step
In two, zinc acetate methanol solution is to disperse in methyl alcohol, to obtain dense by magnetic agitation 2h by the zinc acetate of 0.55g at room temperature
Degree is the zinc acetate methanol solution of 0.5mol/L.
3. the preparation method of Al doping ZnO ultrathin nanometer piece sensitive material according to claim 1, it is characterized in that：Step
In four, digestion solution is by 0.05mol/L zinc nitrate, 0.05mol/L hexamethylenetetramine, 0.05mol/L ammonium hydroxide and 0.002mol/
L polyethyleneimine configures mixed solution, with ultrapure water it is fixed it is molten after to get arriving ZnO digestion solution.
4. the preparation method of Al doping ZnO ultrathin nanometer piece sensitive material according to claim 1, it is characterized in that：Gained
Nanometer sheet is having a size of 1 μm -3 μm, with a thickness of 10nm-30nm.
5. the purposes of the ZnO ultrathin nanometer piece of Al doping obtained by any one of -4 the methods according to claim 1, it is characterized in that：
Gas sensor is prepared as sensitive material.
6. the purposes of the ZnO ultrathin nanometer piece of Al doping according to claim 5, it is characterized in that：The gas sensor is existed
Aging 1-2 days at a temperature of 240-340 DEG C realize the detection to alcohol gas by the variation of control ZnO nano material resistance.
7. the purposes of the ZnO ultrathin nanometer piece of Al doping according to claim 6, it is characterized in that：It is to 100ppm ethyl alcohol
Response be 90, the response-recovery time is respectively less than 2s, and detection is limited to 2ppm.
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| KR20020023821A (en) * | 2001-12-11 | 2002-03-29 | 태원필 | Humidity sensor using Al-doped ZnO thin film |
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Application publication date: 20181130 |