CN105776357A - Method for preparing nickel oxide/zinc oxide heterojunction nanometer materials - Google Patents
Method for preparing nickel oxide/zinc oxide heterojunction nanometer materials Download PDFInfo
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- CN105776357A CN105776357A CN201610160764.6A CN201610160764A CN105776357A CN 105776357 A CN105776357 A CN 105776357A CN 201610160764 A CN201610160764 A CN 201610160764A CN 105776357 A CN105776357 A CN 105776357A
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
The invention discloses a method for preparing nickel oxide/zinc oxide heterojunction nanometer materials. By the aid of the method, the technical problem of low sensitivity of nickel oxide/zinc oxide heterojunction nanometer materials prepared by the aid of existing methods can be solved. The technical scheme includes that the method comprises synthesizing nickel oxide/zinc oxide heterojunction pre-sintered powder from mixed solution by the aid of a one-step hydrothermal process; calcining the nickel oxide/zinc oxide heterojunction pre-sintered powder to obtain the nickel oxide/zinc oxide heterojunction nanometer materials. The mixed solution is prepared from nickel acetate tetrahydrate, zinc nitrate hexahydrate and sodium hydroxide. The method has the advantages that the method only includes one reaction step instead of two reaction steps in the prior art, and the reaction time is shortened and is 12 h instead of the reaction time of 60 h in the prior art; as shown in gas sensitivity tests, the working temperatures of gas sensors made of the nickel oxide/zinc oxide heterojunction nanometer materials prepared by the aid of the method are lowered and are 200 DEG C instead of the working temperatures of 330 DEG C in the prior art; the sensitivity of the gas sensors for 100 ppm acetone gas is improved and reaches 15-17 instead of the sensitivity of 12 in the prior art.
Description
Technical field
The preparation method that the present invention relates to a kind of nano material, particularly to the preparation method of a kind of nickel oxide/ZnO heterojunction nano material.
Background technology
Since entering 21 century, people's environmental pollution and energy shortage problem are increasingly paid close attention to, and the scientific research for these two aspects also gets more and more.Zinc oxide is a kind of common metal-oxide semiconductor (MOS), and owing to it is in many-sided performances such as optical, electrical, magnetics, zinc oxide is widely used in the fields such as photocatalyst, gas sensitive material, dielectric material.Wherein, zinc oxide is a class important in gas sensitive material, it is possible to dusty gas poisonous in environment, harmful is monitored.But, the problems such as zinc oxide gas sensitive sensitivity is low, operating temperature is high, poor selectivity are also problems in the urgent need to address.Therefore, research and development Zinc oxide-base heterojunction nanometer material is effectively easy method for improving sensitivity, reducing operating temperature, improve the air-sensitive performance such as selectivity, equally, also vital effect is played in the industrial processes such as air pollution monitoring and saving cost.
nullDocument " Y.Liu,G.Li,etal.Anenvironment-benignmethodforthesynthesisofp-NiO/n-ZnOheterostructurewithexcellentperformanceforgassensingandphotocatalysis.SensorsandActuatorsB:Chemical,2014,191,537-544. " report employing two step chemical synthesiss be prepared for nickel oxide/ZnO heterojunction nano material，First prepared by zinc nitrate hexahydrate and potassium hydroxide hybrid reaction 12h nano zinc oxide material as carrier，Then zinc oxide is distributed to six water nickel nitrates and reaction 48h in the mixed solution of carbamide，Finally calcine 3h at 400 DEG C and obtain nickel oxide/ZnO heterojunction nano material.Its course of reaction is complicated, the response time up to 60h, simultaneously, its air-sensitive performance has been detected, and result shows that its operating temperature higher is 330 DEG C, and the sensitivity to the acetone gas of 100ppm is 12, its operating temperature is higher, and sensitivity is relatively low is unfavorable for practical application.
Summary of the invention
For the deficiency that the nickel oxide/ZnO heterojunction nano material sensitivity overcoming existing method to prepare is low, the preparation method that the present invention provides a kind of nickel oxide/ZnO heterojunction nano material.The mixed solution that four water nickel acetates, zinc nitrate hexahydrate and sodium hydroxide are made into by the method, nickel oxide/ZnO heterojunction pre-burning powder body is synthesized with one step hydro thermal method, then calcine 1～3h at 300～400 DEG C and obtain nickel oxide/ZnO heterojunction nano material, its reactions steps is reduced to a step by two steps of background technology, and the response time is reduced to 12h by the 60h of background technology；, testing through air-sensitive performance, nickel oxide prepared by the present invention/ZnO heterojunction Nano-meter Materials as Gas Sensors operating temperature is reduced to 200 DEG C by the 330 of background technology DEG C meanwhile；And, its sensitivity of acetone gas of 100ppm is brought up to 15～17 by the 12 of background technology.
The technical solution adopted for the present invention to solve the technical problems: the preparation method of a kind of nickel oxide/ZnO heterojunction nano material, is characterized in comprising the following steps:
Step one, by four water nickel acetates: zinc nitrate hexahydrate: sodium hydroxide 1:4:10～1:19:40 in molar ratio is dissolved completely in distilled water, magnetic agitation 10～20min so that it is become the solution of uniformly clarification；
Step 2, gained solution in step one is transferred to autoclave it is sealed in 80～100 DEG C of reacting by heating 6～18h, it is neutral for product distilled water and dehydrated alcohol cyclic washing being centrifuged to solution ph, products therefrom be placed in baking oven 50～70 DEG C dry 6～10h, obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, by step 2 prepare nickel oxide/zinc oxide pre-burning powder body calcine in Muffle furnace, heating rate is 3～8 DEG C/min, and calcining heat is 300～400 DEG C, and calcination time is 1～3h, obtains nickel oxide/ZnO heterojunction nano material.
The invention has the beneficial effects as follows: the mixed solution that four water nickel acetates, zinc nitrate hexahydrate and sodium hydroxide are made into by the method, nickel oxide/ZnO heterojunction pre-burning powder body is synthesized with one step hydro thermal method, then calcine 1～3h at 300～400 DEG C and obtain nickel oxide/ZnO heterojunction nano material, its reactions steps is reduced to a step by two steps of background technology, and the response time is reduced to 12h by the 60h of background technology；, testing through air-sensitive performance, nickel oxide prepared by the present invention/ZnO heterojunction Nano-meter Materials as Gas Sensors operating temperature is reduced to 200 DEG C by the 330 of background technology DEG C meanwhile；And, its sensitivity of acetone gas of 100ppm is brought up to 15～17 by the 12 of background technology.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of nickel oxide prepared by the embodiment of the present invention 1～3/ZnO heterojunction nano material.
Fig. 2 is nickel oxide prepared by the embodiment of the present invention 2/ZnO heterojunction nano material scanning electron microscopic picture.
Fig. 3 is that the gas sensor of nickel oxide prepared by the embodiment of the present invention 2/ZnO heterojunction nano material is exposed in the acetone steam of 100ppm operating temperature and the response recovery curve of sensitivity.
Fig. 4 is the Sensitivity comparison figure that the gas sensor of nickel oxide prepared by the embodiment of the present invention 1～3/ZnO heterojunction nano material is exposed in the acetone steam of 100ppm when 200 DEG C.
Detailed description of the invention
Following example are with reference to Fig. 1-4.
Embodiment 1:
Step one, by four water nickel acetates: zinc nitrate hexahydrate: sodium hydroxide 1:4:10 in molar ratio is dissolved completely in distilled water, magnetic agitation 10min so that it is become the solution of uniformly clarification；
Step 2, gained solution in step one is transferred to autoclave it is sealed in 80 DEG C of reacting by heating 18h, it is neutral for product distilled water and dehydrated alcohol cyclic washing being centrifuged to solution ph, products therefrom be placed in baking oven 50 DEG C dry 10h, obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, by step 2 prepare nickel oxide/zinc oxide pre-burning powder body calcine in Muffle furnace, heating rate is 3 DEG C/min, and calcining heat is 300 DEG C, and calcination time is 3h, obtains nickel oxide/ZnO heterojunction nano material.
Can be seen that the compound phase that sample is nickel oxide and zinc oxide prepared by embodiment 1 from the X ray diffracting spectrum of Fig. 1 (a), be wherein the characteristic diffraction peak of nickel oxide at (200) crystal face that the angle of diffraction is 43 degree.The sensitivity that the nickel oxide/ZnO heterojunction nano material of embodiment 1 preparation is exposed in the acetone steam of 100ppm when 200 DEG C as can be seen from Figure 4 is brought up to 15 by the 12 of background technology.
Embodiment 2:
Step one, by four water nickel acetates: zinc nitrate hexahydrate: sodium hydroxide 1:9:20 in molar ratio is dissolved completely in distilled water, magnetic agitation 15min so that it is become the solution of uniformly clarification；
Step 2, gained solution in step one is transferred to autoclave it is sealed in 90 DEG C of reacting by heating 12h, it is neutral for product distilled water and dehydrated alcohol cyclic washing being centrifuged to solution ph, products therefrom be placed in baking oven 60 DEG C dry 8h, obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, by step 2 prepare nickel oxide/zinc oxide pre-burning powder body calcine in Muffle furnace, heating rate is 5 DEG C/min, and calcining heat is 350 DEG C, and calcination time is 2h, obtains nickel oxide/ZnO heterojunction nano material.
The compound phase that sample is nickel oxide and zinc oxide prepared by embodiment 2 is can be seen that from the X ray diffracting spectrum of Fig. 1 (b).As can be seen from Figure 2 the zinc oxide of embodiment 2 preparation is shuttle shape structure, and its diameter Distribution is 100～200nm, and nickel oxide nanoparticle is dispersed in zinc oxide surface composition nickel oxide/ZnO heterojunction.As can be seen from Figure 3 100ppm acetone gas is had different response curves by the nickel oxide/ZnO heterojunction nano material of embodiment 2 preparation at different temperatures, wherein there is maximum sensitivity when operating temperature is 200 DEG C, illustrate that the operating temperature of nickel oxide/ZnO heterojunction nano material gas sensor prepared by the present embodiment is reduced to 200 DEG C by the 330 of background technology DEG C.The sensitivity that the nickel oxide/ZnO heterojunction nano material of embodiment 2 preparation is exposed in the acetone steam of 100ppm when 200 DEG C as can be seen from Figure 4 is brought up to 17 by the 12 of background technology.
Embodiment 3:
Step one, by four water nickel acetates: zinc nitrate hexahydrate: sodium hydroxide 1:19:40 in molar ratio is dissolved completely in distilled water, magnetic agitation 20min so that it is become the solution of uniformly clarification；
Step 2, gained solution in step one is transferred to autoclave it is sealed in 100 DEG C of reacting by heating 6h, it is neutral for product distilled water and dehydrated alcohol cyclic washing being centrifuged to solution ph, products therefrom be placed in baking oven 70 DEG C dry 6h, obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, by step 2 prepare nickel oxide/zinc oxide pre-burning powder body calcine in Muffle furnace, heating rate is 8 DEG C/min, and calcining heat is 400 DEG C, and calcination time is 1h, obtains nickel oxide/ZnO heterojunction nano material.
Can be seen that the compound phase that sample is nickel oxide and zinc oxide prepared by embodiment 3 from the X ray diffracting spectrum of Fig. 1 (c), along with the content of nickel oxide reduces, its angle of diffraction also weakens to some extent the characteristic peak intensity of 43 degree.The sensitivity that the nickel oxide/ZnO heterojunction nano material of embodiment 3 preparation is exposed in the acetone steam of 100ppm when 200 DEG C as can be seen from Figure 4 is brought up to 16 by the 12 of background technology.
The preparation method that the invention provides a kind of nickel oxide/ZnO heterojunction nano material, is specially a step hydrothermal synthesis method and prepares nickel oxide/ZnO heterojunction nano material.The method reactions steps is simple, the response time is short, and meanwhile, the gas sensor operating temperature of nickel oxide/ZnO heterojunction nano material is low, and sensitivity improves.Therefore, be conducive to saving cost to be suitable for promoting the use of in the industrial production.
Claims (1)
1. the preparation method of nickel oxide/ZnO heterojunction nano material, it is characterised in that comprise the following steps:
Step one, by four water nickel acetates: zinc nitrate hexahydrate: sodium hydroxide 1:4:10～1:19:40 in molar ratio is dissolved completely in distilled water, magnetic agitation 10～20min so that it is become the solution of uniformly clarification；
Step 2, gained solution in step one is transferred to autoclave it is sealed in 80～100 DEG C of reacting by heating 6～18h, it is neutral for product distilled water and dehydrated alcohol cyclic washing being centrifuged to solution ph, products therefrom be placed in baking oven 50～70 DEG C dry 6～10h, obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, by step 2 prepare nickel oxide/zinc oxide pre-burning powder body calcine in Muffle furnace, heating rate is 3～8 DEG C/min, and calcining heat is 300～400 DEG C, and calcination time is 1～3h, obtains nickel oxide/ZnO heterojunction nano material.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784156A (en) * | 2017-01-05 | 2017-05-31 | 上海芯石微电子有限公司 | One kind is based on NiO/ZnO nanorod heterojunction diodes and preparation method thereof |
| CN107285393A (en) * | 2017-07-13 | 2017-10-24 | 济南大学 | A kind of NiO nanometer sheets/α Fe with triethylamine sensitlzing effect2O3Nanocube heterojunction material |
| CN107715890A (en) * | 2017-11-02 | 2018-02-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of heterogeneous ozone catalyst and products thereof and application |
| CN109019705A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of MOF induces the preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive |
| CN109647414A (en) * | 2019-01-25 | 2019-04-19 | 郑州大学 | NiO-ZnO ball chain shape nano material and its preparation method and application |
| CN110596196A (en) * | 2019-09-16 | 2019-12-20 | 山东大学 | Semiconductor heterojunction gas sensitive material and preparation method and application thereof |
| CN110743555A (en) * | 2019-10-08 | 2020-02-04 | 中国科学院兰州化学物理研究所 | Preparation method of nano porous metal nickel catalyst |
| CN113155907A (en) * | 2021-03-10 | 2021-07-23 | 东北电力大学 | Detection of SF6Decomposition gas H2ZnO-NiO gas sensor of S |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
| CN115072808A (en) * | 2022-06-29 | 2022-09-20 | 西北工业大学 | Nickel molybdate-nickel oxide flower-like microsphere material, preparation method and application thereof, ethanol gas sensor and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784156A (en) * | 2017-01-05 | 2017-05-31 | 上海芯石微电子有限公司 | One kind is based on NiO/ZnO nanorod heterojunction diodes and preparation method thereof |
| CN107285393A (en) * | 2017-07-13 | 2017-10-24 | 济南大学 | A kind of NiO nanometer sheets/α Fe with triethylamine sensitlzing effect2O3Nanocube heterojunction material |
| CN107715890A (en) * | 2017-11-02 | 2018-02-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of heterogeneous ozone catalyst and products thereof and application |
| CN109019705A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of MOF induces the preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive |
| CN109647414A (en) * | 2019-01-25 | 2019-04-19 | 郑州大学 | NiO-ZnO ball chain shape nano material and its preparation method and application |
| CN109647414B (en) * | 2019-01-25 | 2021-12-07 | 郑州大学 | NiO-ZnO spherical chain-shaped nano material and preparation method and application thereof |
| CN110596196A (en) * | 2019-09-16 | 2019-12-20 | 山东大学 | Semiconductor heterojunction gas sensitive material and preparation method and application thereof |
| CN110743555A (en) * | 2019-10-08 | 2020-02-04 | 中国科学院兰州化学物理研究所 | Preparation method of nano porous metal nickel catalyst |
| CN113155907A (en) * | 2021-03-10 | 2021-07-23 | 东北电力大学 | Detection of SF6Decomposition gas H2ZnO-NiO gas sensor of S |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
| CN115072808A (en) * | 2022-06-29 | 2022-09-20 | 西北工业大学 | Nickel molybdate-nickel oxide flower-like microsphere material, preparation method and application thereof, ethanol gas sensor and preparation method thereof |
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