CN109437278A - It is a kind of based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material, preparation process and its application - Google Patents
It is a kind of based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material, preparation process and its application Download PDFInfo
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Abstract
本发明公开了一种基于氧化铜‑氧化锡核壳纳米线结构的气敏纳米材料、制备工艺及其应用。本发明氧化铜核层纳米线的制备采用合成条件极其简单的化学溶液法，结合壳层的原子层沉积技术，得到了氧化铜/氧化锡核壳结构纳米线。与现有制备工艺相比，本发明具有可重复性强，成品率高，制备效率高，可规模化生产等优点。本发明构建的基于p‑n异质结的核壳结构，其应用于气体传感时灵敏度大幅提升，响应时间和恢复时间则大幅缩减，展现了更加优异的气敏性能。本发明的气敏纳米材料能够对微量有机挥发性气体进行检测，并且对甲醛气体具有优异的选择性，为气体监测领域开发高灵敏度、高稳定性的气体传感器提供了坚实的技术支持。
The invention discloses a gas-sensing nanomaterial based on a copper oxide-tin oxide core-shell nanowire structure, a preparation process and an application thereof. The preparation of the copper oxide core layer nanowire of the present invention adopts a chemical solution method with extremely simple synthesis conditions, combined with the atomic layer deposition technology of the shell layer, to obtain the copper oxide/tin oxide core-shell structure nanowire. Compared with the existing preparation process, the invention has the advantages of strong repeatability, high yield, high preparation efficiency, and large-scale production. The core-shell structure based on the p - n heterojunction constructed by the present invention greatly improves the sensitivity when it is applied to gas sensing, and greatly reduces the response time and recovery time, and exhibits more excellent gas sensing performance. The gas-sensing nanomaterial of the invention can detect trace organic volatile gas and has excellent selectivity for formaldehyde gas, which provides solid technical support for the development of a gas sensor with high sensitivity and high stability in the field of gas monitoring.
Description
Technical field
The present invention relates to semiconductor nano material preparation technical field, refer specifically to a kind of there is high-specific surface area, highly sensitive
Degree based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material, preparation process and its is answered with excellent stability
With.
Background technique
In recent years, the resistance-type gas sensor based on semiconductor nano material has been a great concern, extensively
Applied to every field such as gas leakage alarms, monitored gas environment and industrial gasses analyses.It researches and develops and various possesses high-ratio surface
The new gas sensing based on metal oxide semiconductor material of long-pending, excellent gas sorption ability and high carrier mobility
Device has become current research hotspot.In various metal oxide semiconductor materials, copper oxide (CuO) is a kind of excellentp
Type multifunctional semiconductor material, has been widely studied applied to high performance gas sensor.In order to improve copper oxide gas sensing
The performance of device, a large amount of research is dedicated to designing and manufacturing different nanostructures, such as nano wire, nano flower and nanocube
Deng to increase specific surface area, to improve the gas sorption ability of material.
However, a large amount of studies have shown that its air-sensitive performance of the gas sensor based on single copper oxide material is relatively poor.
The preparation of sandwich causes extensive research interest as a result, is generally considered a kind of raising gas sensor
The effective ways of energy.Precious metal doping is a kind of preparation method of sandwich.Since noble metal has superior catalysis
Performance, after the noble metals such as incorporation Ag, Pt and Pd, sensing capabilities are obviously improved semiconductor gas sensor.However, it is contemplated that
The preparation cost of precious metal doping is quite high, and the sensitivity of sensor and service life can be seriously undermined because of poisoning, simultaneously
Noble metal has larger toxicity, can not be with bio-compatible, and application receives apparent limitation.Therefore, a kind of more economical reality
With and widely accepted method be to construct the nucleocapsid heterojunction structure being made of two or more semiconductor materials.
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 copper oxide-tin oxide p-n junction
Air-sensitive nano material, preparation process and its application of core-shell nano cable architecture.The present invention uses advanced technique for atomic layer deposition,
The thickness of film is accurately controlled in atomic level and possesses excellent conformal covering power, there is repeatability by force, yield rate
The advantages that height, preparation efficiency is high is prepare with scale core-shell structure CuO/SnO2Nano wire provides a kind of completely new thinking.This
Invent the CuO/SnO being prepared2Nuclear shell structure nano line has high-specific surface area, high sensitivity, Gao Xuan as gas sensitive
The characteristics of selecting property and excellent stability.
In the present invention, the preparation of the copper oxide stratum nucleare nano wire in nuclear shell structure nano line is extremely simple using synthesis condition
Chemical solution method, the preparation of tin oxide shell uses technique for atomic layer deposition.Technical solution of the invention is specific as follows.
The present invention provide it is a kind of based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material preparation process,
Specific step is as follows:
(1) NaOH and (NH is prepared4)2S2O8Mixed solution, in mixed solution, the concentration of NaOH is 1 ~ 1.5mol/L, (NH4)2S2O8Concentration be 0.05 ~ 0.075 mol/L；
(2) using the foam copper after cleaning-drying as substrate and source material, it is soaked in 10 ~ 15min in mixed solution vertically, soaks
After bubble, foam copper is taken out, foam copper surface grows Cu azury (OH)2Nano wire, deionized water cleaning, drying；
(3) by Cu (OH)2Nano wire from ultrasonic Separation in foam copper substrate, it is evenly dispersed in deionized water, then will obtain
Mass volume ratio is the hanging drop of 1 ~ 5 mg/ml on the quartz plate substrate that standard cleaning is crossed, 50 ~ 80 DEG C of temperature in air
Lower baking is until be completely dried；
(4) Cu (OH) will be coated with2The quartz plate of nano wire 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；
(5) above-mentioned be put into Muffle furnace through the sample that atomic layer deposition is prepared is calcined；After calcining, natural cooling
To room temperature, copper oxide/tin oxide core-shell nano cable architecture air-sensitive nano material is obtained.
In above-mentioned steps (2), being cleaned and dried foam copper includes successively cleaning each ultrasound clearly with dehydrated alcohol and deionized water
After washing 10 ~ 15 min, the step of drying with high pure nitrogen.
In above-mentioned steps (2), after taking out foam copper, successively it is cleaned by ultrasonic respectively 2 ~ 4 times with dehydrated alcohol and deionized water,
2 ~ 3 min of each ultrasound.
In above-mentioned steps (2), the intermediate product Cu (OH) that is prepared2It is about 7 ~ 10 μm of the average length of nano wire, average
Diameter is 110 ~ 150 nm.
In above-mentioned steps (4), 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 (4), during technique for atomic layer deposition deposition film, SnO2The growth rate of film is
0.05 ~ 0.15 nm/ circulation.
In above-mentioned steps (5), calcination procedure are as follows: after being heated to 550 ~ 600 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 made from a kind of above-mentioned preparation process based on copper oxide-tin oxide core-shell nano cable architecture gas
Quick nano material.
The average length of the copper oxide that the present invention obtains-tin oxide core-shell nano cable architecture air-sensitive nano material is 7 ~ 10
μm, average diameter depends on the SnO of atomic layer deposition2Film thickness.Preferably, for if gas sensitive, thickness substantially to exist
20 ~ 28 nm are more excellent
The present invention further provides a kind of based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material in detection first
Application in terms of aldehyde gas.
Compared to the prior art, the beneficial effects of the present invention are:
1, the core-shell structure based on p-n heterojunction is constructed, compared to single copper oxide or single tin oxide structure, is applied to
Sensitivity is substantially improved when gas sensing, and response time and recovery time substantially reduce, and presents more excellent air-sensitive performance.
2, nanowire structure effectively increases the specific surface area of material, further improves the air-sensitive performance of material.
3, copper oxide of the invention/tin oxide core-shell nano cable architecture air-sensitive nano material is to all volatile organic gas
Body has different degrees of response, can be used for monitoring TVOC(volatile organic compounds total amount) concentration；Meanwhile all
In VOCs, the selectivity of PARA FORMALDEHYDE PRILLS(91,95) gas is relatively optimal, and PARA FORMALDEHYDE PRILLS(91,95) gas presents excellent selectivity.
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.
Detailed description of the invention
Fig. 1 is that the present invention is a kind of based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material preparation process
Flow diagram.
Fig. 2 is the scanning electron microscope phenogram for the Kocide SD nano wire that embodiment 1 obtains.
Fig. 3 is copper oxide-tin oxide core-shell nano line scanning electron microscope phenogram that embodiment 1 obtains.
Fig. 4 is copper oxide-tin oxide core-shell nano line Tunneling Microscope phenogram that embodiment 1 obtains.
Fig. 5 is that the C/S-24 core-shell nano line in embodiment 1 carries out gas sensing survey to the formaldehyde gas of 50 ~ 1.5 ppm
Attempt.
Fig. 6 is selective sensing testing figure of the C/S-24 core-shell nano line in embodiment 1 to gas with various.
Specific embodiment
Below in conjunction with drawings and examples, present invention is further described in detail.
A kind of process based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material preparation process of the present invention
Block diagram is as shown in Figure 1.
Embodiment 1
One kind is based onp-nIt includes following for tying the preparation process of copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material
Step:
(1) it takes the Chinese red foam copper that a block size is the cm of 1.5 cm × 3.5 as substrate and source material, is successively soaked in
Respectively it is cleaned by ultrasonic 10 min in dehydrated alcohol and deionized water, is dried up at room temperature with high pure nitrogen.
(2) preparing NaOH concentration is 1.25 mol/L, (NH4)2S2O8The mixed solution that concentration is 0.0625 mol/L is made
For reaction solution.
(3) foam copper after cleaning-drying is soaked in 10 min in above-mentioned reaction solution vertically, successively with anhydrous after taking-up
Ethyl alcohol and deionized water are cleaned by ultrasonic 3 times respectively, wherein 3 min of ultrasound every time, are dried up with high pure nitrogen at room temperature after the completion, steep
It is 8 μm that foam copper surface, which grows light blue average length, and average diameter is the Cu (OH) of 132 nm2Nano wire is (such as Fig. 2 institute
Show).
(4) by the above-mentioned Cu (OH) being prepared2Nano wire is dispersed in from ultrasonic Separation in foam copper substrate
In ionized water, and by obtained mass volume ratio be about 5 mg/ml hanging drop in 2.5 cm × 2.5 that standard cleaning is crossed
On the quartz plate substrate of cm size, 80 DEG C of bakings are until be completely dried in air.
(5) Cu (OH) will be coated with2The quartz plate of nano wire is put into BENEQ TFS-200 ALD reaction chamber, using atom
Layer deposition techniques prepare SnO2Blanket films select four (dimethylamino) tin (TDMASn) wherein setting reaction temperature as 200 DEG C
As tin source, deionized water sets the heating temperature of solid-state tin source TDMASn as 45 DEG C as oxygen source, and sets growth circulation
Number is 240 cycles, wherein the growth course of each circulation includes 0.5 s TDMASn pulse, 10 s N2(g) it purges, 0.2
The pulse of s deionized water and 10 s N2(g) it purges, SnO is prepared2Blanket films are as shown in Figure 2 with a thickness of 24 nm().
(6) 550 DEG C of 2 h of calcining in Muffle furnace are put into through the sample that atomic layer deposition is prepared by above-mentioned, wherein heating up
Rate is 10 DEG C/min.
(7) sample is taken out after Muffle in-furnace temperature cooled to room temperature to get being 8 μ to sepia average length
M, average diameter are that 172 nm(shell thicknesses are 24 nm) copper oxide-tin oxide core-shell nano line (being named as C/S-24) knot
The air-sensitive nano material (as shown in Figure 3) of structure.
Gas sensing test is carried out using formaldehyde gas of the obtained C/S-24 core-shell nano line to 50 ~ 1.5 ppm.To 50
The formaldehyde gas of ppm, the sensitivity (being defined as responsiveness -1) of C/S-24 core-shell nano line are 1.42, and pure CuO nano wire
Sensitivity is 0.48, and core-shell nano cable architecture of the invention will improve 2 times to the sensing sensitivity of 50 ppm formaldehyde gas, right
Formaldehyde gas its sensitivity under other concentration also has different degrees of promotion (as shown in Figure 5).In addition, to obtained C/S-24
Core-shell nano line has carried out selectivity test, i.e., carries out respectively to the formaldehyde of same concentrations (50 ppm), acetone, toluene and ammonia
Gas sensing test.As shown in fig. 6, copper oxide of the invention-tin oxide core-shell nano line PARA FORMALDEHYDE PRILLS(91,95) gas present it is excellent
Selectivity.
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 (10)
1. a kind of preparation process based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material, which is characterized in that
Specific step is as follows:
(1) NaOH and (NH is prepared4)2S2O8Mixed solution, in mixed solution, the concentration of NaOH is 1 ~ 1.5mol/L, (NH4)2S2O8Concentration be 0.05 ~ 0.075 mol/L；
(2) using the foam copper after cleaning-drying as substrate and source material, it is soaked in 10 ~ 15 min in mixed solution vertically, soaks
After bubble, foam copper is taken out, foam copper surface grows Cu azury (OH)2Nano wire, deionized water cleaning, drying；
(3) by Cu (OH)2Nano wire from ultrasonic Separation in foam copper substrate, it is evenly dispersed in deionized water, then the matter that will be obtained
Measuring volume ratio is the hanging drop of 1 ~ 5 mg/ml on the quartz plate substrate that standard cleaning is crossed, in air at a temperature of 50 ~ 80 DEG C
Baking is until be completely dried；
(4) Cu (OH) will be coated with2The quartz plate of nano wire 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；
(5) above-mentioned be put into Muffle furnace through the sample that atomic layer deposition is prepared is calcined；After calcining, natural cooling
To room temperature, copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material is obtained.
2. preparation process as described in claim 1, which is characterized in that in step (2), being cleaned and dried foam copper includes successively using
After dehydrated alcohol 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 (2), after taking out foam copper, successively with anhydrous
Ethyl alcohol and deionized water are cleaned by ultrasonic 2 ~ 4 times respectively, 2 ~ 3 min of each ultrasound.
4. preparation process as described in claim 1, which is characterized in that in step (2), Cu (OH)2The average length of nano wire
It is 7 ~ 10 μm, average diameter is 110 ~ 150 nm.
5. preparation process as described in claim 1, which is characterized in that in step (4), 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.
6. preparation process as described in claim 1, which is characterized in that in step (4), deposited using technique for atomic layer deposition thin
In membrane process, SnO2The growth rate of film is 0.05 ~ 0.15 nm/ circulation.
7. preparation process as described in claim 1, which is characterized in that in step (5), calcination procedure are as follows: with 8 ~ 12 DEG C/min
Heating rate be heated to 550 ~ 600 DEG C after, continue 1 ~ 3 h of heat preservation.
8. a kind of preparation process as described in claim 1 is obtained based on copper oxide-tin oxide core-shell nano cable architecture gas
Quick nano material.
9. as claimed in claim 8 based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material, feature exists
In average length is 7 ~ 10 μm, with a thickness of 20 ~ 28 nm.
10. one kind is as claimed in claim 8 or 9 based on copper oxide-tin oxide core-shell nano cable architecture air-sensitive nano material
Application in terms of detecting formaldehyde gas.
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