CN109019705A - A kind of MOF induces the preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive - Google Patents

A kind of MOF induces the preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive Download PDF

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CN109019705A
CN109019705A CN201810861981.7A CN201810861981A CN109019705A CN 109019705 A CN109019705 A CN 109019705A CN 201810861981 A CN201810861981 A CN 201810861981A CN 109019705 A CN109019705 A CN 109019705A
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mof
zinc oxide
gas sensitive
sheath structure
combined oxidation
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宋鹏
位祺
王�琦
杨中喜
马振壬
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University of Jinan
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/04—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • 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
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • 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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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)

Abstract

The present invention provides a kind of preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive of MOF induction.The preparation method specifically includes: using nickel nitrate and zinc sulfate as raw material, using N-N dimethylformamide (DMF) and polyethylene glycol as solvent, terephthalic acid (TPA) is organic linking agent, using traditional solvent-thermal method, after keeping the temperature 6 h under 150 °C, obtains MOF and induce three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive.This method simple production process, resulting zinc oxide and the compound gas sensitive of nickel oxide have shell sheath and hierarchical structure, have increased considerably the specific surface area of material, obtain highly sensitive novel gas sensitive.

Description

A kind of MOF induces the system of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive Preparation Method
Technical field
The present invention relates to be related to a kind of preparation side of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive of MOF induction Method belongs to advanced nano-functional material fabricating technology field.
Background technique
Into after 21 century, global industry is rapidly developed, and brings huge benefit for the development of the mankind, but same with this When, problem of environmental pollution is also increasingly severe, wherein especially gaseous contamination, not only generates massive losses to social property, together When also can generate huge challenge to the health of the mankind.For example, triethylamine is used as a kind of inflammable and poisonous gas, it can be right Human skin and mucous membrane are irritant, and it is even dead that pulmonary edema can be generated when concentration is higher.Therefore, people increasingly pay attention to having The detection of poisonous gas.For gas detection method there are many, wherein by metal oxide prepare semiconductor gas sensor Due to its high sensitivity, long service life, it is at low cost the advantages that and be widely used.Main metal oxide has SnO2、 ZnO、Fe2O3Deng traditional gas sensitive, also there is In2O3, the novel gas sensitive such as NiO, CuO.That this experiment mainly discusses is ZnO With the air-sensitive performance of NiO.ZnO is a kind of typical N-type semiconductor, and forbidden bandwidth is 3.37 eV, is examined due to having to gas Survey that reversible, the adsorption desorption time is short, physicochemical properties are stable, the advantages that being able to detect multiple gases under preference temperature, but its There are still sensitivity it is relatively low, operating temperature is higher the disadvantages of, therefore be the emphasis of air-sensitive research field for a long time.Oxygen simultaneously Change nickel as a kind of novel p-type gas sensitive, is also had a wide range of applications in air-sensitive field；But due to p-type gas sensitive Sensitivity is lower, therefore how to improve its gas sensing property still up for further studying.
For nano material, the variation of morphosis can generate large effect to the air-sensitive performance of material, no It only can further improve the selectivity of gas sensitive, moreover it is possible to promote its sensitivity further.At present there are many The nanostructured zinc oxide and nickel oxide of form are successfully prepared, as Liu et al. (B. Liu, H. Yang, H. Zhao, Synthesis and enhanced gas-sensing properties of ultralong NiO nanowires Assembled with NiO nanocrystals, Sens. Actuators B, 156 (2011) 251-262.) to super The successful preparation of long NiO nanotube；Jing et al. (Z. Jing, J. Zhan, Fabrication and gas-sensing 20 (2008) 547-4551. of properties of porous ZnO nanoplates, Adv. Mater.) discovery it is porous ZnO nano piece has good gas sensing property to chlorobenzene and ethyl alcohol.In addition, preparing metal semiconductor using the method for MOF induction Method increasingly by the concern of research circle.This method has the characteristics that diversity and easily controllable using the form of organic matter, Organic matter is removed by calcining, obtained oxide is still able to maintain original form and forms porous structure, this is conducive to improve The specific surface area of material, so as to improve its its gas sensing property.For example, Lu et al. (Y. Lu, W. Zhan, Y. He, MOF- templated synthesis of porous Co3O4 concave nanocubes with high specific surface area and their gas sensing properties, ACS Appl. Mater. Interfaces, 6 (2014) 4186-4195.) find the Co that MOF is induced3O4Nanocube has biggish specific surface area and excellent gas sensing property Energy.Since single gas sensitive has certain limitation always, so focus is gradually transferred to composition metal oxygen by people In the preparation of compound gas sensitive.With other metal oxides it is compound after, on the one hand oxidize metal object formed multidimensional classification knot Structure enables gas sensitive to adsorb more test gases to increase the specific surface area of material；On the other hand, different It is capable of forming hetero-junctions between metal oxide, promotes the separation of electronics and hole, accelerates the transmission of electronics, so as to improve material Air-sensitive performance, such as Ju et al. (D. Ju, High triethylamine-sensing properties of NiO/SnO2 hollow sphere P–N heterojunction sensors, Sens. Actuators B 215 (2015) 39- 44.) SnO is had studied2With compound rear influence of the hetero-junctions to air-sensitive performance of NiO.Although pure NiO closes sensitivity of the ZnO to gas It is not very high, but will be helpful to improve its air-sensitive performance by being compounded to form hetero-junctions..
Summary of the invention
The object of the present invention is to provide a kind of MOF to induce three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive Preparation method, this method has that at low cost, easy to operate, yield is high and does not generate noxious material, therefore can be realized industry The large-scale production of change.Obtained MOF induces three-dimensional shell sheath structure zinc oxide combined oxidation nickel to have biggish specific surface area, The absorption for being conducive to gas can be applied to gas sensor field.Realizing the technical solution of the object of the invention is: a kind of MOF Induce the preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive, it is characterised in that: with nickel nitrate and sulfuric acid Zinc is raw material, and using N-N dimethylformamide (DMF) and polyethylene glycol as solvent, terephthalic acid (TPA) is organic linking agent, using biography The solvent-thermal method of system after keeping the temperature 6 h under 150 °C, obtains MOF and induces three-dimensional shell sheath structure zinc oxide combined oxidation nickel air-sensitive Material.Specific step is as follows:
(1) 8 ml N-N dimethylformamides and 5 ml polyethylene glycol are first measured in beaker, 0.015 mol/L six is being added Zinc sulphate hydrate and a certain amount of Nickelous nitrate hexahydrate, wherein the concentration of Nickelous nitrate hexahydrate is 0.01 ~ 0.02 mol/L control The molar ratio of Nickelous nitrate hexahydrate and six zinc sulphate hydrates is (0.7 ~ 1.3): 1；
(2) acquired solution is poured into 50 ml reaction kettles, 5 ~ 7 h is kept the temperature under 130 ~ 170 °C；The precipitating of acquisition uses N- respectively N-dimethylformamide is washed three times, and dehydrated alcohol, which washes twice, (should suitably be dispersed in the process using ultrasonic cleaning machine, and subtracted Less granular agglomeration)；
(3) the centrifugation product that step (2) obtains is poured into surface plate, 60 °C of 6 h of heat preservation in baking oven obtain having for MOF induction Machine product；
(4) sample after drying is put into Muffle furnace under 450 ~ 550 °C by step (3) and calcines 20 min, can be obtained The nanoshell sheath structure of zinc oxide combined oxidation nickel.
Detailed description of the invention
Fig. 1 is the XRD spectrum that MOF induces three-dimensional shell sheath structure zinc oxide combined oxidation nickel.
Fig. 2 is the FESEM figure that MOF induces three-dimensional shell sheath structure zinc oxide combined oxidation nickel.
Fig. 3 is the TEM figure that MOF induces three-dimensional shell sheath structure zinc oxide combined oxidation nickel.
Fig. 4 is that MOF induces three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensor to 20- under optimum operating voltage The sensitivity curve figure of the Triethylamine gas of 500 ppm.
Fig. 5 is the response that MOF induces three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensor under optimum operating voltage Recovery curve.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation Example.
Embodiment 1
(1) 8 ml N-N dimethylformamides and 5 ml polyethylene glycol are first measured in beaker, 0.015 mol/L six is being added Zinc sulphate hydrate and 0.01 mol/L Nickelous nitrate hexahydrate, the molar ratio for controlling Nickelous nitrate hexahydrate and six zinc sulphate hydrates are 0.7:1；
(2) acquired solution is poured into 50 ml reaction kettles, 5 h is kept the temperature under 130 °C；The precipitating of acquisition uses N-N diformazan respectively Base formamide washs three times, and dehydrated alcohol, which washes twice, (should suitably be dispersed in the process using ultrasonic cleaning machine, and reduce particle Agglomeration)；
(3) the centrifugation product that step (2) obtains is poured into surface plate, 60 °C of 6 h of heat preservation in baking oven obtain having for MOF induction Machine product；
(4) sample after drying is put into Muffle furnace under 450 °C by step (3) and calcines 20 min, can be obtained oxidation The nanoshell sheath structure of zinc combined oxidation nickel.
Embodiment 2
(1) 8 ml N-N dimethylformamides and 5 ml polyethylene glycol are first measured in beaker, 0.015 mol/L six is being added Six nitric hydrate of zinc sulphate hydrate and 0.015 mol/L, the molar ratio for controlling Nickelous nitrate hexahydrate and six zinc sulphate hydrates is 1: 1；
(2) acquired solution is poured into 50 ml reaction kettles, 6 h is kept the temperature under 150 °C；The precipitating of acquisition uses N-N diformazan respectively Base formamide washs three times, and dehydrated alcohol, which washes twice, (should suitably be dispersed in the process using ultrasonic cleaning machine, and reduce particle Agglomeration)；
(3) the centrifugation product that step (2) obtains is poured into surface plate, 60 °C of 6 h of heat preservation in baking oven obtain having for MOF induction Machine product；
(4) sample after drying is put into Muffle furnace under 500 °C by step (3) and calcines 20 min, can be obtained oxidation The nanoshell sheath structure of zinc combined oxidation nickel.
Embodiment 3
(1) 8 ml N-N dimethylformamides and 5 ml polyethylene glycol are first measured in beaker, 0.015 mol/L six is being added Zinc sulphate hydrate and 0.02 mol/L Nickelous nitrate hexahydrate, the molar ratio for controlling Nickelous nitrate hexahydrate and six zinc sulphate hydrates are 1.3:1；
(2) acquired solution is poured into 50 ml reaction kettles, 7 h is kept the temperature under 170 °C；The precipitating of acquisition uses N-N diformazan respectively Base formamide washs three times, and dehydrated alcohol, which washes twice, (should suitably be dispersed in the process using ultrasonic cleaning machine, and reduce particle Agglomeration)；
(3) the centrifugation product that step (2) obtains is poured into surface plate, 60 °C of 6 h of heat preservation in baking oven obtain having for MOF induction Machine product；
(4) sample after drying is put into Muffle furnace under 550 °C by step (3) and calcines 20 min, can be obtained oxidation The nanoshell sheath structure of zinc combined oxidation nickel.

Claims (1)

1. a kind of MOF induces the preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive, specific synthesis step It is as follows:
(1) 8 ml N-N dimethylformamides and 5 ml polyethylene glycol are first measured in beaker, 0.015 mol/L six is being added Zinc sulphate hydrate and a certain amount of Nickelous nitrate hexahydrate, wherein the concentration of Nickelous nitrate hexahydrate is 0.01 ~ 0.02 mol/L, control The molar ratio of Nickelous nitrate hexahydrate and six zinc sulphate hydrates is (0.7 ~ 1.3): 1；
(2) acquired solution is poured into 50 ml reaction kettles, 5 ~ 7 h is kept the temperature under 130 ~ 170 °C；The precipitating of acquisition uses N- respectively N-dimethylformamide is washed three times, and dehydrated alcohol, which washes twice, (should suitably be dispersed in the process using ultrasonic cleaning machine, and subtracted Less granular agglomeration)；
(3) the centrifugation product that step (2) obtains is poured into surface plate, 60 °C of 6 h of heat preservation in baking oven obtain having for MOF induction Machine product；
(4) sample after drying is put into Muffle furnace under 450 ~ 550 °C by step (3) and calcines 20 min, can be obtained oxygen Change the nanoshell sheath structure of zinc combined oxidation nickel.
CN201810861981.7A 2018-08-01 2018-08-01 A kind of MOF induces the preparation method of three-dimensional shell sheath structure zinc oxide combined oxidation nickel gas sensitive Pending CN109019705A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110247041A (en) * 2019-06-26 2019-09-17 浙江大学 A kind of ZnNiO/C composite nano materials and preparation method thereof
CN115722229A (en) * 2022-11-04 2023-03-03 中国科学技术大学苏州高等研究院 Bimetal oxide nano material and preparation method and application thereof

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CN105776357A (en) * 2016-03-21 2016-07-20 西北工业大学 Method for preparing nickel oxide/zinc oxide heterojunction nanometer materials
CN107316986A (en) * 2017-05-04 2017-11-03 南京邮电大学 A kind of oxide nano thread MOF derivatives/S composite positive poles and preparation method thereof

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CN101269850A (en) * 2008-05-06 2008-09-24 华东理工大学 Method for preparing flower form nickelous oxide
CN105776357A (en) * 2016-03-21 2016-07-20 西北工业大学 Method for preparing nickel oxide/zinc oxide heterojunction nanometer materials
CN107316986A (en) * 2017-05-04 2017-11-03 南京邮电大学 A kind of oxide nano thread MOF derivatives/S composite positive poles and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110247041A (en) * 2019-06-26 2019-09-17 浙江大学 A kind of ZnNiO/C composite nano materials and preparation method thereof
CN115722229A (en) * 2022-11-04 2023-03-03 中国科学技术大学苏州高等研究院 Bimetal oxide nano material and preparation method and application thereof
CN115722229B (en) * 2022-11-04 2024-02-06 中国科学技术大学苏州高等研究院 Bimetallic oxide nano material and preparation method and application thereof

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