CN106187318A - A kind of preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth - Google Patents
A kind of preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth Download PDFInfo
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- CN106187318A CN106187318A CN201610557204.4A CN201610557204A CN106187318A CN 106187318 A CN106187318 A CN 106187318A CN 201610557204 A CN201610557204 A CN 201610557204A CN 106187318 A CN106187318 A CN 106187318A
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Abstract
The invention discloses the preparation method of the ceramic base Vanadium dioxide nanometer rod structure of a kind of freedom and on-plane surface growth, comprise the following steps: the cleaning of ceramic substrate；Weigh V2O5Powder；Single gas phase transmission sedimentation prepares the step of ceramic base Vanadium dioxide nanometer rod.The invention provides a kind of easy and simple to handle, can the low cost method of preparing ceramic base Vanadium dioxide nanometer rod, the required process conditions controlled of single Vapor Transport are few, and environmentally safe.Further, the ceramic base Vanadium dioxide nanometer rod structure deposited has large specific surface area and gas diffusion paths, is more beneficial for absorption and the diffusion of gas.Result shows, the ceramic base Vanadium dioxide nanometer rod structure prepared by the present invention will reduce methane gas dependent sensor operating temperature, improve the research space that methane gas dependent sensor sensitivity aspect provides the biggest.
Description
Technical field
The present invention relates to the preparation method of a kind of gas sensitive, the ceramic base grown particularly to a kind of freedom and on-plane surface
The controllable method for preparing of Vanadium dioxide nanometer rod structure.
Background technology
Due to methane (i.e. gas, CH4) inflammable and explosive feature, the least spark can cause violent blast, is made
User brings certain danger, detects its concentration in time, has highly important to safety precaution detection and leakage warning
Effect.Therefore, the research of methane gas dependent sensor is necessary.Research currently for methane gas dependent sensor is big
Mostly it is based on widely studied metal oxide semiconductor materials such as zinc oxide, stannum oxide.But these conductor oxidates pass
The operating temperature of sensor is high, and it causes sensor ageing quickening, and stability declines, and power consumption is increased.At present, it is achieved methane
The room temperature high-sensitivity detection of gas remains one and is rich in challenging task.
Vanadium dioxide is the N-type metal oxide semiconductor material of a kind of low energy gap, has had been reported that and has mentioned it to hydrogen
Detection there is higher sensitivity, and can work at room temperature.By vanadium dioxide materials application in methane gas dependent sensor it is
One latest find.A.K.Prasad in 2014 et al. finds that vanadium dioxide has sensitivity characteristic to methane gas, but it is surveyed
Examination operating temperature is 50 DEG C-150 DEG C, and optimum working temperature is 50 DEG C, remains above room temperature.And peak response is 1.4%.This
Outer air-sensitive response recovery time is long.Research shows, think nanostructured have bigger specific surface area, surface activity, with
And stronger gas sorption ability, and then the reaction between gas can be strengthened, effective while improving sensitivity further
Reduce operating temperature.
Summary of the invention
In order to solve problems of the prior art, the present invention provides a kind of freedom and the ceramic base two of on-plane surface growth
The preparation method of vanadium oxide nanorod structure, overcomes current sensor operating temperature high, and structure is complicated, and response recovery time is short,
The problem that can not realize room temperature detection.
The technical scheme is that the system of the ceramic base Vanadium dioxide nanometer rod structure of a kind of freedom and on-plane surface growth
Preparation Method, comprises the following steps:
(1) cleaning of ceramic substrate
Ultrasonic cleaning 5～20min in acetone and ethanol respectively by ceramic substrate, to remove the oil of ceramic substrate surface
Dirt, organic impurities and surface oxide layer, take out ceramic substrate and blow away the liquid of substrate surface, suction with your ball of suction after having cleaned
Be put on filter paper after complete liquid and in the vacuum drying oven of 60～80 DEG C be dried 5-10min standby；
(2) V2O5 powder is weighed
Weigh V2O5 powder standby；
(3) single gas phase transmission sedimentation prepares ceramic base Vanadium dioxide nanometer rod
V by step (2)2O5Powder evaporation source is uniformly laid on the ceramic substrate of step (1), and entirety puts into quartz ampoule
In, then holding V2O5The ceramic bases of a piece of step (1) is placed in the appropriate position of ceramic powder substrate, and quartz ampoule is whole
Body is put in programmable type high-temperature vacuum tubular type furnace apparatus, grows vanadium dioxide with single gas phase transmission sedimentation in tube furnace
Nanometer rods.
The evaporation source V of described step (2)2O5Powder be quality purity be the V of 99.999%2O5Powder.
Described step (3) technological parameter uses using the argon of quality purity 99.999% as working gas, before experiment
Cleaning burner hearth 5～10min, in making stove, vacuum reaches below 20Pa, and then effusion meter is adjusted to " opening " shelves, and institute is tested in regulation
Ar throughput 20sccm needed, regulates operating pressure 1.5Torr, arranges depositing temperature 1000 DEG C, sedimentation time 1-4h, try
Test.
Described step (3) sedimentation time is 3h.
The invention have the benefit that and the invention provides a kind of easy and simple to handle, low cost can prepare ceramic base titanium dioxide
The method of vanadium nanometer rods, the required process conditions controlled of single Vapor Transport are few, and environmentally safe.Further, deposited
Ceramic base Vanadium dioxide nanometer rod structure there is large specific surface area and gas diffusion paths, be more beneficial for gas absorption and
Diffusion.Add grown part nanometer rods be non-planar growth that is depart from plane to outgrowth, these factors make two
Vanadium oxide nanometer rods can fully adsorb the oxygen in air and the reducibility gas CH of needs detection4.Based on vanadium dioxide nano
The methane transducer of rod can effectively realize room temperature high-sensitivity detection methane gas.Result shows, the pottery prepared by the present invention
Porcelain base Vanadium dioxide nanometer rod structure will reduce methane gas dependent sensor operating temperature, improve methane gas dependent sensor sensitivity
Aspect provides the biggest research space.
Accompanying drawing explanation
Fig. 1 is the growth course figure of ceramic base Vanadium dioxide nanometer rod: (a) is V2O5It is grown to the process of droplet, (b)
It is to be grown to VO by mesophase2The process of nanometer rods；
Fig. 2 is the ceramic base Vanadium dioxide nanometer rod surface Scanning Electron microphotograph prepared by embodiment 1；
Fig. 3 is the ceramic base Vanadium dioxide nanometer rod surface Scanning Electron microphotograph prepared by embodiment 2；
Fig. 4 is the ceramic base Vanadium dioxide nanometer rod section Scanning Electron microphotograph prepared by embodiment 2；
Fig. 5 is the ceramic base Vanadium dioxide nanometer rod XRD analysis result photo prepared by embodiment 2；
Fig. 6 is that the ceramic base Vanadium dioxide nanometer rod structure prepared by embodiment 2 is to 100～500ppm CH4Moving of gas
State response curve；
Fig. 7 is the ceramic base Vanadium dioxide nanometer rod surface Scanning Electron microphotograph prepared by embodiment 3；
Fig. 8 is the ceramic base Vanadium dioxide nanometer rod surface Scanning Electron microphotograph prepared by embodiment 4.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in more detail.
The present invention is raw materials used all uses commercially available chemically pure reagent.
Embodiment 1
(1) cleaning of ceramic substrate
By rectangular-shaped, then by a piece of for two panels that the potsherd of a piece of a size of 2cm*2cm cuts into a size of 2cm*1cm
Complete puts in glass with the potsherd after a piece of cutting, ultrasonic cleaning 5～20min in acetone and ethanol respectively, clearly
Take out ceramic substrate after washing and blow away the liquid of substrate surface with inhaling that ball, be put on filter paper after sucking liquid and in 60～
The vacuum drying oven of 80 DEG C is dried 5～10min standby；
(2) V is weighed2O5Powder
Weigh 0.15g V2O5Powder is standby；
(3) single gas phase transmission sedimentation prepares ceramic base Vanadium dioxide nanometer rod
V by step (2)2O5On the ceramic substrate of the 2cm*2cm that powder evaporation source is uniformly laid on step (1), and entirety is put
Enter in quartz ampoule, then hold V in distance2O5At the ceramic substrate 0.5cm of powder, (direction of argon stream) places step (1)
The ceramic substrate of a piece of 2cm*1cm, puts into programmable type high-temperature vacuum tubular type stove (GSL-1400X type) equipment by quartz ampoule entirety
In, using the argon of quality purity 99.999% as working gas, effusion meter is adjusted to " cleaning " shelves, clean burner hearth 5～
10min, is then adjusted to " closedown " shelves by effusion meter, and in making stove, vacuum reaches below 20Pa, then is adjusted to " beat by effusion meter
Open " shelves, Ar throughput 20sccm needed for regulation experiment, regulate operating pressure 1.5Torr, heating curve is set and wherein deposits temperature
Spending 1000 DEG C, sedimentation time 4h, final step occurs that "-121 " are i.e. provided with, tests；
Prepared by embodiment 1 is 1-dimention nano bar structure, freedom and the Vanadium dioxide nanometer rod surface of on-plane surface growth
Topography scan electron-microscopic analysis result is as shown in Figure 2.
Embodiment 2
The present embodiment is with the difference of embodiment 1: in step (3), single Vapor Transport prepares ceramic base dioxy
The sedimentation time changing vanadium nanometer rods is 3h, obtained ceramic base Vanadium dioxide nanometer rod surface and cross-sectional scanning electron microscope
Analysis result is as shown in Figures 3 and 4.The nanometer rods size uniform of the present embodiment, average diameter and a length of 150nm and 23 μm.Institute
The ceramic base Vanadium dioxide nanometer rod XRD analysis result of preparation is as it is shown in figure 5, result shows that vanadium dioxide is monoclinic crystal knot
Structure.
The ceramic base Vanadium dioxide nanometer rod structure gas sensor element prepared by embodiment 2 at room temperature to 100～
The CH of 500ppm4The dynamic response curve of gas is as shown in Figure 6.Image shows that ceramic base Vanadium dioxide nanometer rod structure can be in room
Temperature detects methane gas and has good reversibility.
Embodiment 3
The present embodiment is with the difference of embodiment 1: in step (3), single Vapor Transport prepares ceramic base dioxy
That changes vanadium nanometer rods arranges sedimentation time 2h, and the nanometer rods size deposited is uneven but starts to grow along different directions, presents
Free growing pattern.Obtained ceramic base Vanadium dioxide nanometer rod surface topography scanning electron microscope analysis result such as figure
Shown in 7.
Embodiment 4
The present embodiment is with the difference of embodiment 1: in step (3), single Vapor Transport prepares ceramic base dioxy
That changes vanadium nanometer rods arranges sedimentation time 1h, prepared nanometer rods the most adjacent one-tenth nanometer pencil and mainly giving birth in one direction
Long.Ceramic base Vanadium dioxide nanometer rod surface topography scanning electron microscope analysis result is as shown in Figure 8.
Although above in conjunction with accompanying drawing, invention has been described, but the invention is not limited in above-mentioned being embodied as
Mode, above-mentioned detailed description of the invention is only schematically, is not restrictive, and those of ordinary skill in the art is at this
Under the enlightenment of invention, in the case of without departing from present inventive concept and scope of the claimed protection, it is also possible to make a lot of shape
Formula, within these belong to protection scope of the present invention.
Claims (4)
1. the preparation method of the ceramic base Vanadium dioxide nanometer rod structure of a freedom and on-plane surface growth, it is characterised in that bag
Include following steps:
(1) cleaning of ceramic substrate
Ultrasonic cleaning 5～20min in acetone and ethanol respectively by ceramic substrate, to remove the greasy dirt of ceramic substrate surface, to have
Machine thing impurity and surface oxide layer, take out ceramic substrate and blow away the liquid of substrate surface with your ball of suction, sucking liquid after having cleaned
Be put in after body on filter paper and in the vacuum drying oven of 60～80 DEG C be dried 5-10min standby；
(2) V2O5 powder is weighed
Weigh V2O5 powder standby；
(3) single gas phase transmission sedimentation prepares ceramic base Vanadium dioxide nanometer rod
The V2O5 powder evaporation source of step (2) is uniformly laid on the ceramic substrate of step (1), and entirety is put in quartz ampoule,
Then the ceramic bases of a piece of step (1) is placed in the appropriate position holding V2O5 ceramic powder substrate, quartz ampoule is overall
Put in programmable type high-temperature vacuum tubular type furnace apparatus, in tube furnace, grow vanadium dioxide with single gas phase transmission sedimentation and receive
Rice rod.
The preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth the most according to claim 1,
It is characterized in that, the evaporation source V2O5 powder of described step (2) be quality purity be the V2O5 powder of 99.999%.
The preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth the most according to claim 1,
It is characterized in that, described step (3) technological parameter uses using the argon of quality purity 99.999% as working gas, tests it
Front cleaning burner hearth 5～10min, in making stove, vacuum reaches below 20Pa, and then effusion meter is adjusted to " opening " shelves, regulation experiment
Required Ar throughput 20sccm, regulates operating pressure 1.5Torr, arranges depositing temperature 1000 DEG C, sedimentation time 1-4h, carry out
Test.
The preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth the most according to claim 3,
It is characterized in that, described step (3) sedimentation time is 3h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204805A (en) * | 2019-09-11 | 2020-05-29 | 杭州电子科技大学 | Vanadium dioxide nanowire and preparation method and application thereof |
| CN111519257A (en) * | 2019-06-24 | 2020-08-11 | 上海海事大学 | Preparation method of doped vanadium dioxide micron tube array, vanadium dioxide micron tube array and vanadium dioxide micron tube |
| CN112938893A (en) * | 2021-02-09 | 2021-06-11 | 南方科技大学 | Vanadium dioxide single crystal driver and preparation method and application thereof |
| CN112981530A (en) * | 2021-02-09 | 2021-06-18 | 南方科技大学 | Vanadium dioxide single crystal micro-nanowire and preparation method and application thereof |
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| CN104878360A (en) * | 2015-06-12 | 2015-09-02 | 天津大学 | Preparation method for room-temperature methane gas sensor based on vanadium oxide |
| CN105388191A (en) * | 2015-11-19 | 2016-03-09 | 天津大学 | Preparation method of ceramic-based vanadium oxide nano rod structured room temperature CH4 sensor |
| CN105486723A (en) * | 2015-11-19 | 2016-04-13 | 天津大学 | Preparation method for room temperature NO2 sensor with ceramic-based vanadium oxide nanorod structure |
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2016
- 2016-07-15 CN CN201610557204.4A patent/CN106187318A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878360A (en) * | 2015-06-12 | 2015-09-02 | 天津大学 | Preparation method for room-temperature methane gas sensor based on vanadium oxide |
| CN105388191A (en) * | 2015-11-19 | 2016-03-09 | 天津大学 | Preparation method of ceramic-based vanadium oxide nano rod structured room temperature CH4 sensor |
| CN105486723A (en) * | 2015-11-19 | 2016-04-13 | 天津大学 | Preparation method for room temperature NO2 sensor with ceramic-based vanadium oxide nanorod structure |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111519257A (en) * | 2019-06-24 | 2020-08-11 | 上海海事大学 | Preparation method of doped vanadium dioxide micron tube array, vanadium dioxide micron tube array and vanadium dioxide micron tube |
| CN111519257B (en) * | 2019-06-24 | 2021-01-26 | 上海海事大学 | Preparation method of doped vanadium dioxide micron tube array, vanadium dioxide micron tube array and vanadium dioxide micron tube |
| CN111204805A (en) * | 2019-09-11 | 2020-05-29 | 杭州电子科技大学 | Vanadium dioxide nanowire and preparation method and application thereof |
| CN112938893A (en) * | 2021-02-09 | 2021-06-11 | 南方科技大学 | Vanadium dioxide single crystal driver and preparation method and application thereof |
| CN112981530A (en) * | 2021-02-09 | 2021-06-18 | 南方科技大学 | Vanadium dioxide single crystal micro-nanowire and preparation method and application thereof |
| CN112981530B (en) * | 2021-02-09 | 2022-04-05 | 南方科技大学 | Vanadium dioxide single crystal micro-nanowire and preparation method and application thereof |
| CN112938893B (en) * | 2021-02-09 | 2023-10-17 | 南方科技大学 | Vanadium dioxide monocrystal driver and preparation method and application thereof |
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