CN105776357B - 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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- CN105776357B CN105776357B CN201610160764.6A CN201610160764A CN105776357B CN 105776357 B CN105776357 B CN 105776357B CN 201610160764 A CN201610160764 A CN 201610160764A CN 105776357 B CN105776357 B CN 105776357B
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- 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 present invention relates to a kind of preparation method of nano material, more particularly to a kind of nickel oxide/ZnO heterojunction nanometer
The preparation method of material.
Background technology
Into 21 century since, people's environmental pollution and energy shortage problem are increasingly paid close attention to, for this two side
The scientific research in face is also more and more.Zinc Oxide is a kind of common metal-oxide semiconductor (MOS), because it is in light, electricity, magnetics
Etc. many performances, 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, and poisonous in environment, harmful dusty gass can be monitored.But
Be the problems such as Zinc Oxide gas sensitive sensitivity is low, operating temperature is high, poor selectivity be also in the urgent need to address asking
Topic.Therefore, Zinc oxide-base heterojunction nanometer material is researched and developed for raising sensitivity, reduction operating temperature, raising selectivity
It is effectively easy method Deng air-sensitive performance, equally, also air pollution monitoring and the industrial processes such as cost-effective is played
Vital effect.
Document " Y.Liu, G.Li, et al.An environment-benign method for the synthesis
of p-NiO/n-ZnO heterostructure with excellent performance for gas sensing and
photocatalysis.Sensors and Actuators B:Chemical, 2014,191,537-544. " reports employing
Two step chemical synthesiss are prepared for nickel oxide/ZnO heterojunction nano material, first mix zinc nitrate hexahydrate with potassium hydroxide
Reaction 12h prepares nano zinc oxide material as carrier, then Zinc Oxide is distributed to into six water nickel nitrates molten with the mixing of carbamide
48h is reacted in liquid, finally 3h is calcined at 400 DEG C and is obtained nickel oxide/ZnO heterojunction nano material.Its course of reaction is complicated,
Response time is up to 60h, meanwhile, its air-sensitive performance is detected, as a result show that its operating temperature is more a height of 330 DEG C, and
Sensitivity to the acetone gas of 100ppm is 12, and its operating temperature is higher, and sensitivity is relatively low to be unfavorable for practical application.
The content of the invention
It is low in order to overcome the shortcomings of nickel oxide/ZnO heterojunction nano material sensitivity prepared by existing method, this
It is bright that a kind of preparation method of nickel oxide/ZnO heterojunction nano material is provided.The method is by four water nickel acetates, zinc nitrate hexahydrate
The mixed solution being made into sodium hydroxide, with one step hydro thermal method nickel oxide/ZnO heterojunction pre-burning powder body, Ran Hou are synthesized
300～400 DEG C of 1～3h of calcining obtain nickel oxide/ZnO heterojunction nano material, its reactions steps by background technology two steps
A step is reduced to, the response time is reduced to 12h by the 60h of background technology；Meanwhile, the test of Jing air-sensitive performances, prepared by the present invention
Nickel oxide/ZnO heterojunction Nano-meter Materials as Gas Sensors operating temperature is reduced to 200 DEG C by 330 DEG C of background technology；And
And, its sensitivity to the acetone gas of 100ppm brings up to 15～17 by the 12 of background technology.
The technical solution adopted for the present invention to solve the technical problems：A kind of nickel oxide/ZnO heterojunction nano material
Preparation method, be characterized in comprising the following steps：
Step one, by four water nickel acetates:Zinc nitrate hexahydrate:Sodium hydroxide in molar ratio 1:4:10～1:19:40 is completely molten
Solution in distilled water, 10～20min of magnetic agitation so as to become the solution of uniform clarification；
Step 2, resulting solution in step one is transferred to autoclave be sealed in 80～100 DEG C of reacting by heating 6～
18h, it is neutral that product distilled water and dehydrated alcohol cyclic washing are centrifuged to solution ph, and products therefrom is placed in 50 in baking oven
～70 DEG C of 6～10h of drying, obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, nickel oxide obtained in step 2/Zinc Oxide pre-burning powder body is calcined in Muffle furnace, heating rate
For 3～8 DEG C/min, calcining heat is 300～400 DEG C, and calcination time is 1～3h, obtains nickel oxide/ZnO heterojunction nanometer
Material.
The invention has the beneficial effects as follows：The mixing that the method is made into four water nickel acetates, zinc nitrate hexahydrate and sodium hydroxide
Solution, with one step hydro thermal method nickel oxide/ZnO heterojunction pre-burning powder body is synthesized, and is then calcined 1～3h at 300～400 DEG C and is obtained
To nickel oxide/ZnO heterojunction nano material, its reactions steps is reduced to a step by two steps of background technology, the response time by
The 60h of background technology is reduced to 12h；Meanwhile, Jing air-sensitive performances test, nickel oxide/ZnO heterojunction prepared by the present invention is received
Rice material gas sensor operating temperature is reduced to 200 DEG C by 330 DEG C of background technology；And, the acetone gas to 100ppm
Its sensitivity brings up to 15～17 by the 12 of background technology.
The present invention is elaborated with reference to the accompanying drawings and detailed description.
Description of the drawings
Fig. 1 is the X-ray diffractogram of nickel oxide prepared by the embodiment of the present invention 1～3/ZnO heterojunction nano material
Spectrum.
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 to
Operating temperature and the response recovery curve of sensitivity in the acetone steam of 100ppm.
Fig. 4 is the gas sensor of nickel oxide prepared by the embodiment of the present invention 1～3/ZnO heterojunction nano material 200
DEG C when be exposed to Sensitivity comparison figure in the acetone steam of 100ppm.
Specific embodiment
Following examples reference picture 1-4.
Embodiment 1：
Step one, by four water nickel acetates：Zinc nitrate hexahydrate：Sodium hydroxide in molar ratio 1:4:10 are dissolved completely in distilled water
In, magnetic agitation 10min so as to become the solution of uniform clarification；
Step 2, resulting solution in step one is transferred to autoclave it is sealed in 80 DEG C of reacting by heating 18h, by product
It is neutral to be centrifuged to solution ph with distilled water and dehydrated alcohol cyclic washing, and products therefrom is placed in 50 DEG C of drying 10h in baking oven,
Obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, nickel oxide obtained in step 2/Zinc Oxide pre-burning powder body is calcined in Muffle furnace, heating rate
For 3 DEG C/min, calcining heat is 300 DEG C, and calcination time is 3h, obtains nickel oxide/ZnO heterojunction nano material.
Can be seen that sample prepared by embodiment 1 is answering for nickel oxide and Zinc Oxide from the X ray diffracting spectrum of Fig. 1 (a)
Phase is closed, wherein in the characteristic diffraction peak that (200) crystal face that the angle of diffraction is 43 degree is nickel oxide.As can be seen from Figure 4 embodiment 1 is made
The sensitivity that standby nickel oxide/ZnO heterojunction nano material is exposed in the acetone steam of 100ppm at 200 DEG C is by carrying on the back
The 12 of scape technology bring up to 15.
Embodiment 2：
Step one, by four water nickel acetates：Zinc nitrate hexahydrate：Sodium hydroxide in molar ratio 1:9:20 are dissolved completely in distilled water
In, magnetic agitation 15min so as to become the solution of uniform clarification；
Step 2, resulting solution in step one is transferred to autoclave it is sealed in 90 DEG C of reacting by heating 12h, by product
It is neutral to be centrifuged to solution ph with distilled water and dehydrated alcohol cyclic washing, and products therefrom is placed in 60 DEG C of drying 8h in baking oven,
Obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, nickel oxide obtained in step 2/Zinc Oxide pre-burning powder body is calcined in Muffle furnace, heating rate
For 5 DEG C/min, calcining heat is 350 DEG C, and calcination time is 2h, obtains nickel oxide/ZnO heterojunction nano material.
Can be seen that sample prepared by embodiment 2 is answering for nickel oxide and Zinc Oxide from the X ray diffracting spectrum of Fig. 1 (b)
Close phase.As can be seen from Figure 2 the Zinc Oxide that prepared by embodiment 2 is fusiform structure, and its diameter Distribution is 100～200nm, is aoxidized
Nano nickel particles are dispersed in zinc oxide surface composition nickel oxide/ZnO heterojunction.As can be seen from Figure 3 embodiment 2
The nickel oxide of preparation/ZnO heterojunction nano material has at different temperatures different responses bent to 100ppm acetone gas
Line, wherein there is the sensitivity of maximum when operating temperature is 200 DEG C, illustrates nickel oxide manufactured in the present embodiment/zinc oxide heterogeneous
The operating temperature of knot nano material gas sensor is reduced to 200 DEG C by 330 DEG C of background technology.Embodiment 2 as can be seen from Figure 4
The nickel oxide of preparation/ZnO heterojunction nano material be exposed at 200 DEG C the sensitivity in the acetone steam of 100ppm by
The 12 of background technology bring up to 17.
Embodiment 3：
Step one, by four water nickel acetates：Zinc nitrate hexahydrate：Sodium hydroxide in molar ratio 1:19:40 are dissolved completely in distillation
In water, magnetic agitation 20min so as to become the solution of uniform clarification；
Step 2, resulting solution in step one is transferred to autoclave it is sealed in 100 DEG C of reacting by heating 6h, by product
It is neutral to be centrifuged to solution ph with distilled water and dehydrated alcohol cyclic washing, and products therefrom is placed in 70 DEG C of drying 6h in baking oven,
Obtain nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, nickel oxide obtained in step 2/Zinc Oxide pre-burning powder body is calcined in Muffle furnace, heating rate
For 8 DEG C/min, calcining heat is 400 DEG C, and calcination time is 1h, obtains nickel oxide/ZnO heterojunction nano material.
Can be seen that sample prepared by embodiment 3 is answering for nickel oxide and Zinc Oxide from the X ray diffracting spectrum of Fig. 1 (c)
Phase is closed, as the content of nickel oxide is reduced, its angle of diffraction has also weakened in 43 degree of feature peak intensity.As can be seen from Figure 4
Nickel oxide/ZnO heterojunction nano material prepared by embodiment 3 is exposed to the spirit in the acetone steam of 100ppm at 200 DEG C
Sensitivity brings up to 16 by the 12 of background technology.
The invention provides a kind of preparation method of nickel oxide/ZnO heterojunction nano material, specially a step hydro-thermal
Synthetic method prepares nickel oxide/ZnO heterojunction nano material.The method reactions steps are simple, the response time is short, meanwhile, oxidation
The gas sensor operating temperature of nickel/ZnO heterojunction nano material is low, and sensitivity is improved.Therefore, be conducive to cost-effective suitable
Conjunction is promoted the use of in the industrial production.
Claims (1)
1. the preparation method of a kind 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 in molar ratio 1:4:10～1:19:40 are dissolved completely in
In distilled water, 10～20min of magnetic agitation so as to become the solution of uniform clarification；
Step 2, resulting solution in step one is transferred to autoclave it is sealed in 80～100 DEG C of 6～18h of reacting by heating, will
It is neutral that product distilled water and dehydrated alcohol cyclic washing are centrifuged to solution ph, and products therefrom is placed in 50～70 DEG C in baking oven
6～10h of drying, obtains nickel oxide/ZnO heterojunction pre-burning powder body；
Step 3, nickel oxide obtained in step 2/Zinc Oxide pre-burning powder body is calcined in Muffle furnace, heating rate is 3
～8 DEG C/min, calcining heat is 300～400 DEG C, and calcination time is 1～3h, obtains nickel oxide/ZnO heterojunction nanometer material
Material.
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| 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 |
| CN107715890B (en) * | 2017-11-02 | 2019-12-03 | 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 |
| 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 |
| CN110596196B (en) * | 2019-09-16 | 2020-09-18 | 山东大学 | Semiconductor heterojunction gas sensitive material and preparation method and application thereof |
| CN110743555B (en) * | 2019-10-08 | 2021-08-13 | 中国科学院兰州化学物理研究所 | Preparation method of nano porous metal nickel catalyst |
| CN113433171B (en) * | 2021-06-24 | 2022-11-22 | 兰州大学 | Gas sensitive material, gas sensor and preparation method and application of gas sensitive material |
| 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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| CN100576577C (en) * | 2008-09-19 | 2009-12-30 | 武汉大学 | A kind of n-ZnO nano wire/p-NiO diode of heterogenous pn junction and preparation method thereof |
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