CN109709192A - It is a kind of based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material, preparation process and its application - Google Patents
It is a kind of based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material, preparation process and its application Download PDFInfo
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Abstract
The invention discloses a kind of based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material, preparation process and its application.The present invention has obtained tungsten oxide/tin oxide nuclear shell structure nano piece in conjunction with technique for atomic layer deposition synthesizing tin oxide layer using a kind of solvent-thermal method preparation oxidation tungsten nucleation layer nanometer sheet that is relatively simple, can in high volume synthesizing.Compared with existing preparation process, the present invention has repeatability strong, high yield rate, and preparation efficiency is high, can large-scale production the advantages that.The present invention construct based onn‑nThe Core-shell structure material combination MEMS of hetero-junctions, sensitivity is substantially improved when as gas sensor, and response time and recovery time substantially reduce, and can be in complex environment to ammonia (NH3) gas have excellent selectivity, can for gas-monitoring field exploitation high sensitivity, high stability gas sensor solid technical support be provided.
Description
Technical field
Sheet material preparation technical field is received the present invention relates to semiconductor, specifically, is related to a kind of based on tungsten oxide/oxidation
Air-sensitive nano material, preparation process and its application of tin core-shell nano chip architecture.
Background technique
In order to meet the needs of interconnection automation and increasingly developed Intelligent internet of things (IoT) device, manufacture is efficiently, surely
Fixed, inexpensive, low-power consumption gas sensor is the direction of an important and worth research.Based on MEMS (MEMS) skill
The chemical-electrical resistive gas sensor of art is in various aspects such as monitoring gas leakage, air quality, food safety and medical diagnosis
Have low-power consumption, micromation and it is integrated many advantages, such as, cause the great research interest of people.In general, MEMS formula
The sensitive material of gas sensor is mostly metal-oxide semiconductor (MOS), such as zinc oxide (ZnO), tungsten oxide (WO3), iron oxide
(Fe2O3) and tin oxide (SnO2) etc..Wherein, the WO of different structure3Nano material, including nanometer rods, mesoporous and nanometer sheet etc.,
Since it is good with chemical stability, responsiveness is high, the advantages such as low in cost, environmentally friendly, gas has been widely used in it
In body sensor.Especially WO3Nanometer sheet and nano wire are since synthesis technology is simple and large specific surface area, in hydrogen sulfide (H2S),
Ammonia (NH3) and nitrogen dioxide (NO2) gas sensing in show excellent performance.In addition to WO3Nano material carries out shape
Looks regulation is outer, and there are also numerous studies based on by adulterating and constructing and the sides such as the composite construction of other metal-oxide semiconductor (MOS)s
Formula improves gas sensing response rate and selectivity.This WO3The enhancing of Quito component material air-sensitive performance is primarily due to
Heterojunction boundary forms depletion layer, promotes electron exchange.
Had received widespread attention in the method for improving gas sensing ability by constructing different core-shell nanostructure and
Research it is advantageous that the material property of stratum nucleare and shell is combined, and constructs double depletion layers between stratum nucleare and shell.Text
The core-shell nano material applied to gas sensor for offering report has ZnO@SnO2, Fe2O3@NiO and CuO@ZnO etc..In addition, gathering around
HavenThe SnO of type characteristic of semiconductor2It is one of traditional gas sensitive, since it is with environmental-friendly, at low cost, resourceful, raw
The characteristics such as object compatibility and thermal stability are good and be concerned.For example, passing through the processing synthesis of two one-step hydrothermal combination subsequent anneals
Sea urchin shape SnO2/α-Fe2O3Heterogeneous Composite nanostructure presents high response characteristic to dimethyl disulfide.Due to gathering around
There are above-mentioned characteristic, SnO2It is had been a great concern as shell in gas sensing field.In view of the gas of nano core-shell material
Quick performance is strongly depend on the thickness of shell, therefore a kind of synthetic method for reasonably capableing of precise thickness control will become raising
The key factor of gas sensor performance.There are many thin-film-coating methods to be applied to SnO at present2The system of blanket films
It is standby, including hydro-thermal method, infusion method, spin-coating method and atomic layer deposition (ALD) method.In these methods, ALD technique is a kind of efficient
The technology for reliably preparing the blanket films of thickness controllable precise, even if under cryogenic, remaining on high aspect ratio structure
The extremely uniform and good conformality thin layer of covering.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide one kind to be based on tungsten oxide/tin oxide nucleocapsid
Air-sensitive nano material, preparation process and its application of nanometer chip architecture.The present invention uses advanced technique for atomic layer deposition, in original
Child level accurately controls the thickness of film and possesses excellent conformal covering power, has repeatability by force, high yield rate, system
The advantages that standby high-efficient is prepare with scale core-shell structure WO3/SnO2Nanometer sheet provides a kind of completely new thinking.And it combines micro-
Mechatronic Systems has obtained the extremely low gas sensor device of power consumption.The tungsten oxide that the present invention is prepared/tin oxide core-shell nano
Piece can be realized based on the gas sensor device that MEMS obtains carries out accurate measurements to ammonia concentration in environment.
In the present invention, WO in core-shell nano piece3Nanometer sheet synthesis work is relatively easy, and the preparation of tin oxide shell uses atom
Layer deposition techniques.Technical solution of the invention is specific as follows.
The present invention provides a kind of preparation work based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material
Skill, the specific steps are as follows:
(1) by 1.0-3.0 g H2WO4It is dissolved in 24-60 milliliters of hydrogen peroxide, obtains with 1.0-3.0 g PVAC polyvinylalcohol
WO3Seed layer spin coating solution；
(2) by WO3Seed layer spin coating solution is uniformly spin-coated under 1000-2500 revs/min of speed by way of spin coating
In clean quartz glass substrate；
(3) under air conditions, by the quartz glass plate after spin coating in Muffle furnace, 400-500 DEG C of temperature lower calcination 1-3 is small
When；
(4) by 0.02 ~ 0.08 mol/L H of 3-6 ml2WO4Solution, 0.02-0.05 g oxalic acid, 0.02-0.04 g urea,
It is mixed to obtain solvent thermal growth for 12.5-35 g acetonitrile solution and the fully dispersed uniform mixing of 6.0 mol/L HCl of 0.5-1.0 ml
Liquid is closed, is then transferred in polytetrafluoroethyllining lining；
(5) quartz glass plate that step (3) obtains is tipped upside down in solvent thermal growth mixed liquor, then tightens stainless steel sleeve
It is transferred to reaction 1-6 hours in 150-180 DEG C of baking oven；
(6) after solvent thermal reaction, obtained sample is washed and dried with deionized water, then in 490 ~ 510 DEG C of temperature
Lower calcining 1-3 hours, growth, which is prepared, WO3The quartz plate of nanometer sheet；
(7) growth there is into WO3The quartz plate of nanometer sheet is put into the reaction chamber of atomic layer deposition thin film system, using atomic layer
Deposition technique prepares SnO2Blanket films select four (dimethylamino) tin wherein setting reaction temperature as 180 ~ 220 DEG C
TDMASn sets the heating temperature of solid-state tin source TDMASn as 45 ~ 50 DEG C as oxygen source as tin source, deionized water；
(8) step (7) is put into Muffle furnace through the sample that atomic layer deposition is prepared and is calcined；It is naturally cold after calcining
But to room temperature, tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material is obtained.
In above-mentioned steps (2), cleaning quartz glass includes successively cleaning each ultrasonic cleaning with dehydrated alcohol and deionized water
After 10 ~ 15 min, the step of drying with high pure nitrogen.
In above-mentioned steps (6), the WO that is prepared3The single-sheet thickness of nanometer sheet is 10-40 nanometers；WO3Nanometer sheet is vertically given birth to
It grows on quartz plate.
In above-mentioned steps (7), the growth course of each circulation includes 0.5 s TDMASn pulse, 10 s N2(g) it purges,
0.2 s deionized water pulse and 10 s N2(g) it purges.
In above-mentioned steps (7), during technique for atomic layer deposition deposition film, SnO2The growth rate of film is
0.05 ~ 0.15 nm/ circulation.
In above-mentioned steps (8), calcination procedure are as follows: after being heated to 450 ~ 550 DEG C with the heating rate of 8 ~ 12 DEG C/min, after
Continue insurance 1 ~ 3 h of temperature.
The present invention also provides a kind of use, and tungsten oxide/tin oxide core-shell nano chip architecture is based on made from above-mentioned preparation process
Air-sensitive nano material.Preferably, single-sheet thickness is 20-100 nanometers, and average thickness depends on the SnO of atomic layer deposition2It is thin
Film thickness.
The present invention further provides a kind of above-mentioned based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nanometer material
Expect the application in terms of detecting ammonia.
In the present invention, before carrying out air-sensitive performance test, first by the tungsten oxide being prepared/tin oxide core-shell nano piece from stone
Scraped on English substrate, it is evenly dispersed in deionized water, and taken appropriate (0.1-0.5 g/ml) drop with heating function
MEMS device on.After the gas sensitive in MEMS heating plate is completely dried at room temperature, device is put into convection oven
Middle 30-60 DEG C 10-24 hours dry.
Compared to the prior art, the beneficial effects of the present invention are:
1, the core-shell structure based on n-n hetero-junctions is constructed, compared to single tungsten oxide or single tin oxide structure, application
Sensitivity is substantially improved when gas sensing, and response time and recovery time substantially reduce, and presents more excellent gas sensing property
Energy.
2, nanometer chip architecture effectively increases the specific surface area of material, further improves the air-sensitive performance of material.
3, tungsten oxide of the invention/tin oxide core-shell nano chip architecture air-sensitive nano material can be to micro (ppm grades)
Volatile organic compounds are detected, and excellent selectivity is presented to ammonia.
4, preparation process of the invention combines technique for atomic layer deposition with the simple chemical solution method of synthesis condition, with
The advantages that conventional preparation techniques, which are compared, has repeatability strong, and high yield rate, preparation efficiency is high, is suitble to prepare with scale
5, the present invention combines micro-electromechanical technology that can substantially reduce the power consumption of gas sensor device and the volume of sensor component.
Detailed description of the invention
Fig. 1 be the present invention it is a kind of based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material preparation and
The flow diagram of gas sensor device preparation technology.
Fig. 2 is tungsten oxide/tin oxide core-shell nano piece scanning electron microscope phenogram that embodiment 1 obtains.
Fig. 3 is tungsten oxide/tin oxide core-shell nano piece transmission electron microscope phenogram that embodiment 1 obtains.
Fig. 4 is the MEMS gas being prepared based on tungsten oxide/tin oxide core-shell nano piece that embodiment 1 obtains
Sensor component figure.
Fig. 5 is the obtained tungsten oxide/tin oxide core-shell nano piece of embodiment 1 to various concentration ammonia sensing capabilities.
Fig. 6 is the obtained tungsten oxide/tin oxide core-shell nano piece of embodiment 1 to ammonia gas selectivity test.
Specific embodiment
Below in conjunction with drawings and examples, present invention is further described in detail.
A kind of process based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material preparation process of the present invention
Block diagram is as shown in Figure 1.
Embodiment 1
A kind of preparation process based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material, the specific steps are as follows:
(1) WO is prepared3Seed layer spin coating solution: 1.0 g H2WO440 milliliters of dioxygens are dissolved in 1.0 g polyvinyl alcohol (PVA)
Water (H2O2) in obtain solution A；
(2) then that solution A is equal under 1000 revs/min of speed by way of spin coating by the supersound washing of quartz glass substrate bottom
Even is spin-coated on clean quartz glass；
(3) under air conditions, by the quartz glass plate after spin coating in Muffle furnace temperature lower calcination 3 hours of 500 DEG C；
(4) H is prepared2WO4Solution, the H2WO4The concentration of solution is 0.05 M, which is used as the source W of solvent thermal growth；
(5) solvent thermal growth mixed liquor is prepared, by 3 ml, 0.05 mol/L H2WO4Solution, 0.02 g oxalic acid, 0.02 g urine
Element, 12.5 g acetonitrile solutions and 0.5 ml HCl(6.0 M) fully dispersed uniform mixing, it is then transferred to the polytetrafluoro of 25 ml
In ethylene liner；
(6) quartz substrate obtained after spin coating before is tipped upside down in growth solution, stainless steel sleeve is then tightened into transfer
It is reacted 2.5 hours in 180 DEG C of baking ovens;
(7) obtained sample is slowly washed and dried with deionized water after solvent thermal reaction, finally by 500 DEG C
High-temperature calcination in 2 hours, WO3The preparation of nano-chip arrays material is completed, and single-sheet thickness is in 30 rans, the width of monolithic nanometer sheet
Degree is 20-80 nanometers, and nanometer sheet grows to obtain perpendicular to quartz substrate；
(8) growth there is into WO3The quartz plate of nanometer sheet is put into the reaction chamber of atomic layer deposition thin film system, using atomic layer
Deposition technique prepares SnO2Blanket films select four (dimethylamino) tin TDMASn to make wherein setting reaction temperature as 180 DEG C
For tin source, deionized water sets the heating temperature of solid-state tin source TDMASn as 45 DEG C as oxygen source, the circulation that control ALD reacts
Tungsten oxide/tin oxide core-shell nano sheet material of different-thickness can be prepared in number；
(9) (heating rate 10 at a temperature of 500 DEG C is put into Muffle furnace through the sample that atomic layer deposition is prepared by above-mentioned
DEG C/min) calcining 2h；After calcining, cooled to room temperature obtains tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive
Nano material, control ALD cycle number is respectively 50,100,200,300 times, has been obtained with a thickness of 32,42,60,81 nanometers
Tungsten oxide/tin oxide core-shell nano sheet material (Fig. 2).When ALD cycle number is 300, obtaining nano thickness is 81 nanometers, from
TEM(Fig. 3) figure can clearly observe core-shell structure.
In order to carry out air-sensitive performance test, by the tungsten oxide being prepared/tin oxide core-shell nano piece from quartz substrate
Scrape, it is evenly dispersed in deionized water, and taken appropriate (0.3 g/ml) drop in the MEMS device with heating function
(Fig. 4 a).MEMS device is connected (Fig. 4 b) by wire bonder with pcb board external circuit, the gas sensitive in MEMS heating plate
After being completely dried at room temperature, device is put into convection oven drying 24 hours at a temperature of 50 DEG C, can be obtained complete
Gas sensor device (as illustrated in fig. 4 c).
The SnO of ALD deposition2Shell thickness has tungsten oxide/tin oxide core-shell nano piece gas sensing performance apparent
Regulating and controlling effect, SnO2Thickness is too thick or too thin sensing characteristics that can all influence core-shell material.Work as SnO2With a thickness of 20 nanometers of left sides
When right, the tungsten oxide/tin oxide core-shell nano piece thickness senses the ammonia gas of 5-50 ppm special at 50-60 nanometers
Property is optimal.The result shows that having reached 2.55 to the response of 50 ppm, resistance change rate is pure WO3Nano sheet material
7.5 times of material.Furthermore selectivity test has been carried out to tungsten oxide/tin oxide core-shell nano chip architecture, i.e., respectively to same concentrations
Ammonia, formaldehyde, acetone, toluene and the hydrogen sulfide of (15 ppm) have carried out gas sensing test.As shown in fig. 6, oxygen of the invention
Change tungsten/tin oxide core-shell nano piece and presents excellent selectivity to ammonia gas.
Embodiments of the present invention are described in detail in above embodiments, and still, present invention is not limited to the embodiments described above
In detail, within the scope of the technical concept of the present invention, can with various simple variants of the technical solution of the present invention are made,
These simple variants all belong to the scope of protection of the present invention.
Claims (9)
1. a kind of preparation process based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material, which is characterized in that
Specific step is as follows:
(1) by 1.0-3.0 g H2WO4It is dissolved in 24-60 milliliters of hydrogen peroxide, obtains with 1.0-3.0 g PVAC polyvinylalcohol
WO3Seed layer spin coating solution；
(2) by WO3Seed layer spin coating solution is uniformly spin-coated under 1000-2500 revs/min of speed by way of spin coating
In clean quartz glass substrate；
(3) under air conditions, by the quartz glass plate after spin coating in Muffle furnace, 400-500 DEG C of temperature lower calcination 1-3 is small
When；
(4) by 0.02 ~ 0.08 mol/L H of 3-6 ml2WO4Solution, 0.02-0.05 g oxalic acid, 0.02-0.04 g urea,
It is mixed to obtain solvent thermal growth for 12.5-35 g acetonitrile solution and the fully dispersed uniform mixing of 6.0 mol/L HCl of 0.5-1.0 ml
Liquid is closed, is then transferred in polytetrafluoroethyllining lining；
(5) quartz glass plate that step (3) obtains is tipped upside down in solvent thermal growth mixed liquor, then tightens stainless steel sleeve
It is transferred to reaction 1-6 hours in 150-180 DEG C of baking oven；
(6) after solvent thermal reaction, obtained sample is washed and dried with deionized water, then in 490 ~ 510 DEG C of temperature
Lower calcining 1-3 hours, growth, which is prepared, WO3The quartz plate of nanometer sheet；
(7) growth there is into WO3The quartz plate of nanometer sheet is put into the reaction chamber of atomic layer deposition thin film system, using atomic layer deposition
Product technology prepares SnO2Blanket films select four (dimethylamino) tin TDMASn to make wherein setting reaction temperature as 180 ~ 220 DEG C
For tin source, deionized water sets the heating temperature of solid-state tin source TDMASn as 45 ~ 50 DEG C as oxygen source；
(8) step (7) is put into Muffle furnace through the sample that atomic layer deposition is prepared and is calcined；It is naturally cold after calcining
But to room temperature, tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material is obtained.
2. preparation process as described in claim 1, which is characterized in that in step (2), cleaning quartz glass includes successively using nothing
After water-ethanol and deionized water clean 10 ~ 15 min of each ultrasonic cleaning, the step of drying with high pure nitrogen.
3. preparation process as described in claim 1, which is characterized in that in step (6), the WO that is prepared3The monolithic of nanometer sheet
With a thickness of 10-40 nanometers；WO3Nanometer sheet vertical-growth is on quartz plate.
4. preparation process as described in claim 1, which is characterized in that in step (7), the growth course of each circulation includes
0.5 s TDMASn pulse, 10 s N2(g) it purges, 0.2 s deionized water pulse and 10 s N2(g) it purges.
5. preparation process as described in claim 1, which is characterized in that in step (7), deposited using technique for atomic layer deposition thin
In membrane process, SnO2The growth rate of film is 0.05 ~ 0.15 nm/ circulation.
6. preparation process as described in claim 1, which is characterized in that in step (8), calcination procedure are as follows: with 8 ~ 12 DEG C/min
Heating rate be heated to 450 ~ 550 DEG C after, continue 1 ~ 3 h of heat preservation.
7. a kind of preparation process as described in claim 1 is obtained based on tungsten oxide/tin oxide core-shell nano chip architecture gas
Quick nano material.
8. air-sensitive nano material as claimed in claim 7, which is characterized in that it is with a thickness of 20-100 nanometers.
9. one kind is being examined based on tungsten oxide/tin oxide core-shell nano chip architecture air-sensitive nano material as claimed in claim 7
Survey the application in terms of ammonia.
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| CN110511059A (en) * | 2019-07-11 | 2019-11-29 | 江苏大学 | Tungstic acid air-sensitive membrane material, tungstic acid base composite air-sensitive membrane material, preparation method and application |
| CN110589875A (en) * | 2019-09-17 | 2019-12-20 | 复旦大学 | Gas-sensitive nano material based on single-layer ordered tin oxide nano bowl branched zinc oxide nanowire structure, preparation process and application thereof |
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| CN114166902A (en) * | 2021-12-07 | 2022-03-11 | 上海大学 | Preparation method of limited-area hydrogen sensor |
| CN114166902B (en) * | 2021-12-07 | 2023-10-20 | 上海大学 | Preparation method of finite field type hydrogen sensor |
| CN114324496A (en) * | 2021-12-20 | 2022-04-12 | 复旦大学 | Gas-sensitive nanomaterial based on Pt particle modified tin oxide/zinc oxide core-shell nanosheet structure, preparation process and application thereof |
| CN114804191A (en) * | 2022-05-12 | 2022-07-29 | 上海复纯环保科技有限公司 | Gas-sensitive nano material based on core-shell structure niobium oxide/tin oxide heterogeneous nanorod, preparation process and application thereof |
| CN114804191B (en) * | 2022-05-12 | 2023-05-12 | 上海复纯环保科技有限公司 | Gas-sensitive nano material based on core-shell structure niobium oxide/tin oxide heterogeneous nanorod, preparation process and application thereof |
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