CN106198867B - A kind of ZnNb2O6The synthetic method of gas sensitive - Google Patents
A kind of ZnNb2O6The synthetic method of gas sensitive Download PDFInfo
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- CN106198867B CN106198867B CN201610516641.1A CN201610516641A CN106198867B CN 106198867 B CN106198867 B CN 106198867B CN 201610516641 A CN201610516641 A CN 201610516641A CN 106198867 B CN106198867 B CN 106198867B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of simple preparation ZnNb2O6The method of gas sensitive, this method utilize hydro-thermal method synthesis ZnNb2O6Presoma, then high-temperature calcination obtain ZnNb2O6 nano materials.The more simple ZnO material gas-selectively of metal oxide, sensitivity are substantially improved, and solve the problem of metal oxide poor selectivity.The advantages of this method, which is to combine by hydro-thermal and high-temperature calcination, prepares high-performance gas sensitive, and the stable performance of material, gas-selectively is good, has broad application prospects.
Description
Technical field
The present invention relates to gas sensor technology field, in particular to a kind of semi-conducting material gas sensitive of excellent performance
Preparation method.
Background technology
Metal oxide such as ZnO, SnO2、WO3Deng because with excellent performance, environment is friendly, aboundresources, cheap
The advantages that, it is the relatively broad gas sensitive of research.But metal oxide has response to majority of gas, by building not
Same structure, the metal oxide of crystal formation can improve sensitivity, response/recovery time etc., but the problem of poor selectivity is difficult to
It is resolved.
The air-sensitive performance of material can be lifted by techniques such as metal oxide composite, surface modifications, in gas sensing
There is very extensive application in device field, and transition metal oxide obtains wide model as important decorative material in terms of material modification
Using bibliography " the Enhanced gas-sensing performance of of the work such as Q. Sun, A.K. Diao
SnO2/Nb2O5hybrid nanowires”（Rsc Advances 2016,6:105317-105321）It is right after adulterating to elaborate
The influence of the performances such as the band gap of semi-conducting material, surface topography is to lifting the sensitivity of material, selectivity has very important shadow
Ring, Nb2O5Doping can introduce more Lacking oxygens.The bibliography of the works such as S. Furukawa, T. Shishido
“Photocatalytic Oxidation of Alcohols over TiO2 Covered with Nb2O5”（ACS Catal.
2012, 2:175-179）, bibliography " the Sol-Gel Derived ZnO of the work such as G.S. Devi, P.S.P. Reddy:
Nb2O5 Nanocomposite as Selective Hydrogen (H2) Gas Sensor”（Materials Today:
Proceedings, 2016, 3: 224 – 229）All elaborate can be substantially improved the light of material as excellent doped chemical
Catalytic performance, air-sensitive performance.But utilize the ZnNb of hydro-thermal method synthesis air-sensitive excellent performance2O6（ZnO：Nb2O5 mol ratios 1:1）
There is not been reported for nano material, and the present invention prepares ZnNb using hydro-thermal method2O6Nano material, material is lifted using high-temperature calcination
Crystallinity, the gas selection characteristic of sensitive material is substantially improved, and improves reactivity and the response time of material, therefore can be with
Improve sensitivity, response time and the selectivity of gas sensitive.
The content of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of processability of simple possible excellent metal oxide
The method of gas sensitive, ZnNb is synthesized using hydro-thermal method2O6Presoma, its crystal property is lifted using high-temperature roasting, can greatly be carried
The selectivity and stability of metal oxide are risen, this method preparation technology is simple, metal oxide system material is passed in air-sensitive
Sensor field has more wide application prospect.
A kind of ZnNb2O6The synthetic method of gas sensitive, it is characterised in that it comprises the following steps：
Step 1：Ethylene glycol and deionized water are pressed 1:0.2-5 volume ratio premix composition mixed solution, adds urea
Regulate and control pH value as subsequent reactions and surfactant is provided；
Step 2：By zinc salt：Acetic acid niobium mol ratio 1:1 carries out dispensing, is added in mixed liquor made from step 1, passes through
Magnetic force heating stirrer stirring at normal temperature is to whole dissolvings, and then 40-80 DEG C is stirred 0.5-1 hours；
Step 3：The solution being stirred is placed in reactor, 90-130 DEG C of reaction 3-8 hour, by gained precipitation second
After alcohol and deionized water cleaning, drying；
Step 4：Dried sample is put into calcining 1-5 hours in Muffle furnace, calcining heat is 600-800 DEG C, is obtained
ZnNb2O6Gas sensitive.
The concentration of described urea is 0.1-0.5M in step 1, and the concentration is the concentration in last mixing liquid.
Described zinc salt is zinc nitrate in step 2, or zinc acetate, or the mixing of the two, and the mol ratio of zinc salt and urea is
0.5-2:1。
Embodiment
Embodiment 1：
40mL ethylene glycol and 10mL deionized water is taken to be placed in beaker, the urea for weighing 10mmol adds above-mentioned mixing
In solution, stirring treats that urea dissolves；The acetic acid niobium of the zinc nitrate and 5mmol that weigh 5mmol is placed in above-mentioned mixed solution, dissolving
Beaker is heated to 60 DEG C afterwards, above-mentioned solution is placed in reactor after stirring 30min, 95 DEG C are reacted 7 hours, and gained is precipitated
Sample is put into Muffle furnace into 700 DEG C with respectively cleaning 3 times of ethanol and deionized water, after drying to calcine 3 hours, obtains ZnNb2O6Gas
Quick material.
Powder made from the present embodiment is scattered to be applied on six pin earthenware air-sensitive testing elements, using WS-30A type air-sensitives
234.7 are reached to acetone gas sensitivity during element test system testing gas concentration 100ppm.
Embodiment 2：
40mL ethylene glycol and 10mL deionized water is taken to be placed in beaker, the urea addition for weighing 7.5mmol is above-mentioned molten
In liquid, stirring treats that urea dissolves；The acetic acid niobium of the zinc nitrate and 5mmol that weigh 5mmol is placed in above-mentioned mixed solution, after dissolving
Beaker is heated to 50 DEG C, above-mentioned solution is placed in reactor after stirring 30min, 120 DEG C are reacted 6 hours, and gained is precipitated
Sample is put into Muffle furnace into 750 DEG C with respectively cleaning 3 times of ethanol and deionized water, after drying to calcine 3 hours, obtains ZnNb2O6Gas
Quick material.
Powder made from the present embodiment is scattered to be applied on six pin earthenware air-sensitive testing elements, using WS-30A type air-sensitives
198.5 are reached to acetone gas sensitivity during element test system testing gas concentration 100ppm.
Embodiment 3：
10mL ethylene glycol and 40mL deionized water is taken to be placed in beaker, the urea for weighing 7.5mmol adds ethylene glycol
In, stirring treats that urea dissolves；The acetic acid niobium of the zinc nitrate and 5mmol that weigh 8mmol is placed in beaker, is heated beaker after dissolving
To 80 DEG C, stir 30min after above-mentioned solution is placed in reactor, 90 DEG C react 8 hours, by gained precipitation ethanol and go from
Respectively cleaning 3 times of sub- water, sample is put into Muffle furnace 700 DEG C after drying and calcined 2 hours, obtains ZnNb2O6Gas sensitive.
Powder made from the present embodiment is scattered to be applied on six pin earthenware air-sensitive testing elements, using WS-30A type air-sensitives
214.6 are reached to acetone gas sensitivity during element test system testing gas concentration 100ppm.
Embodiment 4：
20mL ethylene glycol and 30mL deionized water is taken to be placed in beaker, the urea for weighing 20mmol adds ethylene glycol
In, stirring treats that urea dissolves；The acetic acid niobium of the zinc acetate and 15mmol that weigh 15mmol is placed in beaker, is added beaker after dissolving
Above-mentioned solution is placed in reactor by heat to 50 DEG C after stirring 40min, and 100 DEG C are reacted 6 hours, by gained precipitation ethanol and
Deionized water respectively cleaning 3 times, sample is put into Muffle furnace 650 DEG C after drying and calcined 5 hours, obtains ZnNb2O6Gas sensitive.
Powder made from the present embodiment is scattered to be applied on six pin earthenware air-sensitive testing elements, using WS-30A type air-sensitives
173.4 are reached to acetone gas sensitivity during element test system testing gas concentration 100ppm.
Claims (3)
- A kind of 1. ZnNb2O6The synthetic method of gas sensitive, it is characterised in that it comprises the following steps：Step 1：Ethylene glycol and deionized water are pressed 1:0.2-5 volume ratio premix composition mixed solution, adds urea conduct Subsequent reactions regulate and control pH value and provide surfactant；Step 2：By zinc salt：Acetic acid niobium mol ratio 1:1 carries out dispensing, is added in mixed liquor made from step 1, passes through magnetic force Heating stirrer stirring at normal temperature is to whole dissolvings, and then 40-80 DEG C is stirred 0.5-1 hours；Step 3：The solution being stirred is placed in reactor, 90-130 DEG C of reaction 3-8 hour, by gained precipitation ethanol and After deionized water cleaning, drying；Step 4：Dried sample is put into calcining 1-5 hours in Muffle furnace, calcining heat is 600-800 DEG C, is obtained ZnNb2O6Gas sensitive.
- A kind of 2. ZnNb according to claim 12O6The synthetic method of gas sensitive, it is characterised in that described in step 1 The concentration of urea be 0.1-0.5M, the concentration is the concentration in last mixing liquid.
- A kind of 3. ZnNb according to claim 12O6The synthetic method of gas sensitive, it is characterised in that described in step 2 Zinc salt be zinc nitrate, or zinc acetate, or the mixing of the two, the mol ratio of zinc salt and urea is 0.5-2:1.
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| CN106770495A (en) * | 2016-12-08 | 2017-05-31 | 云南大学 | A kind of high selectivity methyl alcohol gas sensitive and preparation method and application |
| CN107601564B (en) * | 2017-09-04 | 2019-06-07 | 北京工业大学 | A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere |
| CN107991343B (en) * | 2017-11-27 | 2020-07-14 | 哈尔滨学院 | Composite nano semiconductor material AZO/Nb2O5Pt gas sensor and preparation method thereof |
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| CN103570068B (en) * | 2013-10-17 | 2015-11-11 | 陕西科技大学 | A kind of niobite structure ZnNb 2o 6fiber and preparation method thereof |
| CN105502497A (en) * | 2015-12-18 | 2016-04-20 | 中科院微电子研究所昆山分所 | Preparation method for ZnNb2O6 microwave dielectric ceramic powder |
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