CN105129836A - Preparation method for needle-like semiconductor gas-sensitive sensing material - Google Patents
Preparation method for needle-like semiconductor gas-sensitive sensing material Download PDFInfo
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- CN105129836A CN105129836A CN201510509133.6A CN201510509133A CN105129836A CN 105129836 A CN105129836 A CN 105129836A CN 201510509133 A CN201510509133 A CN 201510509133A CN 105129836 A CN105129836 A CN 105129836A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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Abstract
The invention relates to a preparation method for a needle-like semiconductor gas-sensitive sensing material. The method comprises the following steps: putting a copper wire mesh into an acidic solution for immersion and further for removing an oxide layer on the surface, and then performing ultrasonic cleaning on the copper wire mesh by successively using acetone, ethanol and deionized water; putting the copper wire mesh into an alkaline mixed solution containing hydroxyl radical and persulfate ion for reacting for 20-40 min, cleaning for 4-6 times by using deionized water, and drying, so as to obtain a needle-like copper-hydroxide-coated copper wire mesh; performing high-temperature treatment on the composite mesh of which the surface is coated with the blue substance copper hydroxide and the inner layer is copper at 150-200 DEG C for 20-40 min, so as to obtain a copper wire mesh of which the surface is coated with micro-nano needle-like structural copper hydroxide; and putting the micro-nano structural composite copper wire mesh into an ethanol solution for ultrasonic processing for 15-30 min, getting the suspension, and volatilizing ethanol, so as to obtain a black copper oxide powder with relatively high gas-sensitive responsiveness. The raw materials are easy to obtain, the preparation flow is simple, and the prepared gas-sensitive sensing material possesses good selectivity and stability.
Description
Technical field
The present invention relates to the preparation method of a kind acicular semiconductor gas sensing materials, belong to sensing material preparing technical field.
Background technology
Gas sensor is applied widely in environmental monitoring, daily life and commercial process, as by Concentration Testing to methane, carbon monoxide, hydrogen, and can the generation of the effective Peril Incident such as pre-blast protection; As passed through can to provide foundation for the early diagnosis treatment of some disease or cancer to the trace analysis of characteristics of contaminated respiratory droplets gaseous constituent; As the freshness by accurately can judge fish to the odoriferous analysis of fish; As by the gaseous product analysis to Industrial processes, can realize automatically-monitored.
Gas sensor refers generally to target analytes and gas sensing materials interacts, and the change of the physicochemical property of this process is converted into electrical signal by gas sensing device and exports.The Metal Oxide Semiconductor Gas Sensing sensing material with micro-nano structure obviously has following advantage: one, metal oxide semiconductor material raw material is easy to get, the change of physicochemical property can sensitive reaction in change in electric, the output of electrical signal is directly able to simple realization by the change of semi-conductor electricity resistance; Its two, the gas sensitive with micro-nano structure has large specific surface area and hole, and this is conducive to effective diffusion of adsorb oxygen and target analytes, also can provide more nucleation centers on surface be conducive to improve response intensity.The salient features characteristic index of gas sensor has response intensity, selectivity, time of response, time of recovery and stability.Have response intensity high, selectivity is good, and the time of response is fast, and time of recovery is short, and the gas sensitive of permanent stability has broad application prospects.
Summary of the invention
The preparation method of the class acicular semiconductor gas sensing materials that the object of the present invention is to provide a kind of method simple, practical.Cleaned copper mesh is immersed in alkaline mixed solution by the present invention, then adopts the method for thermal treatment and supersound process to obtain the black oxidation copper powder with high gas-sensitive activity.
The preparation method of one kind acicular semiconductor gas sensing materials, is characterized in that the method comprises the following steps:
A. the pre-treatment of copper mesh: copper mesh is put into the oxide skin that acidic solution soaks removing surface, then copper mesh is used successively acetone, ethanol, deionized water ultrasonic cleaning, make copper mesh surface cleaning, be easy to the formation of following micro-nano class acicular structure;
B. the formation of micro-nano class acicular structure: the alkaline mixed solution put into by copper mesh containing hydroxide radical and persulfate ion reacts 20-40min, after question response, the copper mesh of former yellow becomes blueness, by washed with de-ionized water 4-6 time, place seasoning in air, obtain the copper mesh of class needle-like copper hydroxide parcel;
C. the thermal treatment of complex network: will blue material copper hydroxide, internal layer be coated with still for the complex network of copper material is at 150-200 DEG C of pyroprocessing 20-40min, the copper hydroxide pyrolysis making its surface is cupric oxide, thus obtains the copper mesh being coated with micro-nano class acicular structure cupric oxide;
D. the stripping of micro-nano air-sensitive constituent element: what obtained by step C puts into the ultrasonic 15-30min of ethanolic soln containing micro-nano structure compound copper mesh, gets suspension, after ethanol is evaporated completely, must have the black oxidation copper powder of higher air-sensitive responsiveness.
Described alkaline mixed solution is sodium hydroxide and Potassium Persulphate, and its molar concentration rate is 20:1.
The mean diameter of described class needle-like cupric oxide is 0.15-0.17 μm, and length is 3-6 μm.
Getting above-mentioned black CuO powder is placed in slide glass substrate, with Terpineol 350 or deionized water and above-mentioned powder is fully mixed stirs, form the slurry with certain viscosity, then be evenly spin-coated in the vitrified pipe substrate that provided by Zhengzhou Wei Sheng Electronic Technology Co., Ltd, this gas sensing constituent element is placed one week under 60-80 DEG C of condition, surveys its gas-sensitive property.Wherein the blending ratio of black CuO powder and Terpineol 350 or deionized water is 0.006g:30 μ L.
Compared with prior art, the invention has the advantages that:
1, raw material of the present invention is easy to get, and preparation flow is simple, and without the need to relying on expensive equipment, overall cost is low.
2, the gas sensing materials prepared of the present invention, has response and time of recovery faster, all in 30s to benzene.
3, the gas sensing materials prepared of the present invention, having good selectivity, is four times of benzene to the response value of phenyl aldehyde.
4, the present invention has satisfactory stability, and after 30 days, response value remains on more than 90%.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the copper hydroxide covering copper mesh of the embodiment of the present invention 1 gained, and wherein the magnification of a figure is 10000 times, and the magnification of b figure is 50000 times.
Fig. 2 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 gained thermal treatment rear oxidation copper covers copper mesh, and wherein the magnification of a figure is 500 times, and the magnification of b figure is 10000 times.
Fig. 3 is the transmission electron microscope picture of the embodiment of the present invention 1 gained class acicular substance cupric oxide.
Fig. 4 is that the embodiment of the present invention 1 gained cupric oxide gas sensing materials contrasts the respondent behavior (square) of different concns acetone and common cupric oxide powder (trilateral), and wherein concentration unit is ppm.
Fig. 5 is the selectivity test result of the embodiment of the present invention 1 gained class needle-like cupric oxide gas sensing materials.
Fig. 6 is that the embodiment of the present invention 1 gained class needle-like cupric oxide gas sensing materials (a figure) and common cupric oxide powder (b figure) contrasted the time of response of 100ppm benzene and time of recovery.
Embodiment
embodiment 1
(1) pre-treatment of copper mesh:
The hydrochloric acid soln (50mL) original copper mesh being put into 0.1M soaks 50-70s, to remove the oxide skin on surface.Use acetone, ethanol, deionized water supersound process 10min afterwards successively, to remove the various impurity of substrate surface attachment, use deionized water rinsing afterwards three times, purify its surface, then dry up with nitrogen;
(2) formation of class acicular structure:
The copper mesh of gained in step (1) is put into following alkaline mixed solution, the volumetric molar concentration of NaOH is 1M, the volumetric molar concentration of Potassium Persulphate is 0.05M, volume is 50mL, allow it react 30min, after question response, the copper mesh of former yellow becomes blueness, by washed with de-ionized water four times, then dry up with nitrogen.Fig. 1 is the stereoscan photograph that the micro-nano class acicular structure copper hydroxide obtained covers copper mesh.
(3) thermal treatment of complex network:
To be coated with blue material copper hydroxide, internal layer is still for the complex network of copper material is placed in following condition: temperature is 150 DEG C, the time is 30min.The copper hydroxide pyrolysis on its surface is made to be cupric oxide.Still keep original micro-nano class acicular structure simultaneously.After Fig. 2 is the thermal treatment obtained, micro-nano class needle-like cupric oxide covers the stereoscan photograph of copper mesh.
(4) stripping of micro-nano air-sensitive constituent element:
The preparation obtained by step (3) had micro-nano class acicular structure black compound copper mesh to put into ethanolic soln, ultrasonic 30min, gets suspension, after ethanol is evaporated completely, there is the black oxidation copper powder of higher air-sensitive responsiveness.Fig. 3 is the black oxidation copper powder transmission electron microscope photo of this step gained.
(5) spin coating of cupric oxide gas sensitive and air-sensitive performance are tested:
Getting the black powder that 0.006g step (4) obtains is placed in slide glass substrate, with 30 μ L deionized waters and the fully mixed stirring of above-mentioned powder, form the compound with certain viscosity, be then spin-coated in vitrified pipe substrate, vitrified pipe substrate is provided by Zhengzhou Wei Sheng Electronic Technology Co., Ltd.Then this gas sensitive devices to be placed in 60 DEG C of baking ovens one week, to improve its stability.Survey its respondent behavior to different concns acetone, as shown in Figure 4, compared with common cupric oxide, its response intensity has had the raising of highly significant to result.Survey its gas-sensitive property to different sorts gas, its response value as shown in Figure 5, shows good selectivity to phenyl aldehyde.Survey it to the time of response of benzene and time of recovery, as shown in Figure 6, time of response and the time of recovery of class needle-like cupric oxide gas sensing materials are all less than common copper oxide material to result.
embodiment 2
(1) pre-treatment of copper mesh:
The dilute sulphuric acid acid solution (30mL) original copper mesh being put into 0.05M soaks 50s, to remove the oxide skin on surface.Use acetone successively afterwards, ethanol, deionized water supersound process 15min, to remove the organic and inorganic pollutant of original copper net surface attachment, use deionized water rinsing afterwards 3 times, seasoning.
(2) formation of class acicular structure:
The copper mesh of gained in step (1) is put into following alkaline mixed solution, and the volumetric molar concentration of NaOH is 1M, and the volumetric molar concentration of Potassium Persulphate is 0.05M, volume is 40mL, allows it react 20min, after question response, the copper mesh of former yellow becomes blueness, by washed with de-ionized water 3 times, and seasoning.
(3) thermal treatment of complex network:
The copper hydroxide of step (2) gained is covered copper mesh and does following process, temperature is 180 DEG C, and the time is set to 20min.The copper hydroxide pyrolysis on its surface is made to be cupric oxide.
(4) stripping of micro-nano air-sensitive constituent element:
The preparation obtained by step (3) had the substrate of class acicular structure black compound copper mesh to put into ethanolic soln, ultrasonic 25min, gets suspension, after ethanol evaporation is complete, there is the black oxidation copper powder of higher air-sensitive responsiveness.
(5) spin coating of cupric oxide gas sensitive:
Getting the black powder that 0.006g step (4) obtains is placed in slide glass substrate, with 30 μ L deionizations with above-mentioned powder is fully mixed stirs, forms the mashed prod with certain viscosity, is then spin-coated in vitrified pipe substrate.Then this gas sensitive devices to be placed in 80 DEG C of baking ovens one week, to improve its stability.
embodiment 3
(1) process of original copper mesh:
The dilute nitric acid solution (30mL) copper mesh of business being put into 0.05M soaks 30-35s, and fresh copper surface is exposed.Then use acetone successively, ethanol, deionized water supersound process 8-10min, to remove substrate surface dirt settling, dry up with nitrogen again with deionized water rinsing afterwards.
(2) formation of class acicular structure:
The copper mesh of gained in step (1) is placed in the alkaline mixed solution of sodium hydroxide and Potassium Persulphate, volumetric molar concentration is for being followed successively by 1M and 0.05M, volume is 40mL, it is allowed to react 40min, the copper mesh of former yellow becomes blue copper mesh after completion of the reaction, by washed with de-ionized water three times, then seasoning.
(3) thermal treatment of complex network:
The copper mesh covered by copper hydroxide is by following condition pyroprocessing, and temperature is set to 200 DEG C, and the time is set to 20min.Its surface mass pyrolysis is made to be cupric oxide.Still keep original micro-nano class acicular structure simultaneously.
(4) stripping of micro-nano air-sensitive constituent element:
The micro-nano structure cupric oxide covering copper mesh that has obtained by above-mentioned steps is put into ethanolic soln, and ultrasonic 30min, gets suspension, after ethanol is evaporated completely, can have the black oxidation copper powder of higher air-sensitive responsiveness.
(5) spin coating of CuO gas sensitive:
Getting the black powder that about 0.006g step (4) obtains is placed in slide glass substrate, with 30 μ L deionizations with above-mentioned powder is fully mixed stirs, forms the mashed prod with certain viscosity, is then spin-coated in vitrified pipe substrate.The vitrified pipe afterwards this being scribbled cupric oxide gas sensitive is placed in 80 DEG C of next weeks of condition, to improve its stability.
Claims (3)
1. the preparation method of a kind acicular semiconductor gas sensing materials, is characterized in that the method comprises the following steps:
A. the pre-treatment of copper mesh: copper mesh is put into the oxide skin that acidic solution soaks removing surface, then copper mesh is used successively acetone, ethanol, deionized water ultrasonic cleaning;
B. the formation of micro-nano class acicular structure: the alkaline mixed solution put into by copper mesh containing hydroxide radical and persulfate ion reacts 20-40min, then uses washed with de-ionized water 4-6 time, is drying to obtain the copper mesh of class needle-like copper hydroxide parcel;
C. the thermal treatment of complex network: will blue material copper hydroxide, internal layer be coated with still for namely the complex network of copper material obtains the copper mesh being coated with micro-nano class acicular structure cupric oxide at 150-200 DEG C of pyroprocessing 20-40min;
D. the stripping of micro-nano air-sensitive constituent element: what obtained by step C puts into the ultrasonic 15-30min of ethanolic soln containing micro-nano structure compound copper mesh, gets suspension, after ethanol is evaporated completely, obtains black oxidation copper powder.
2. the method for claim 1, it is characterized in that described alkaline mixed solution is sodium hydroxide and Potassium Persulphate, its molar concentration rate is 20:1.
3. the method for claim 1, it is characterized in that the mean diameter of described class needle-like cupric oxide is 0.15-0.17 μm, length is 3-6 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879371A (en) * | 2017-11-17 | 2018-04-06 | 许昌学院 | A kind of method in copper-based material surface in situ growth needle-like Kocide SD |
| GB2613689A (en) * | 2021-11-30 | 2023-06-14 | Univ Xian Architectur & Tech | CuO nanowire-loaded copper mesh and preparation method and use thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879371A (en) * | 2017-11-17 | 2018-04-06 | 许昌学院 | A kind of method in copper-based material surface in situ growth needle-like Kocide SD |
| GB2613689A (en) * | 2021-11-30 | 2023-06-14 | Univ Xian Architectur & Tech | CuO nanowire-loaded copper mesh and preparation method and use thereof |
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