CN106167274A - A kind of preparation method of the Indium sesquioxide. nano-particle with loose structure - Google Patents

A kind of preparation method of the Indium sesquioxide. nano-particle with loose structure Download PDF

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CN106167274A
CN106167274A CN201610571610.6A CN201610571610A CN106167274A CN 106167274 A CN106167274 A CN 106167274A CN 201610571610 A CN201610571610 A CN 201610571610A CN 106167274 A CN106167274 A CN 106167274A
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loose structure
indium
nano
lauryl amine
indium sesquioxide
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CN106167274B (en
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张苏
宋鹏
李嘉
王�琦
杨中喜
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University of Jinan
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    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00Compounds of gallium, indium or thallium
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004Gaseous mixtures, e.g. polluted air
    • G01N33/0009General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
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    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

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Abstract

The invention provides the preparation method of a kind of Indium sesquioxide. nano-particle with loose structure.This preparation method specifically includes: with indium chloride and lauryl amine as raw material, through hydro-thermal reaction, calcination processing, obtain the Indium sesquioxide. nano-particle with loose structure.This method production technology is simple, does not use the surfactant of costliness, and cost ratio is relatively low, and gained Indium sesquioxide. can be as gas sensitive, owing to having loose structure.PARA FORMALDEHYDE PRILLS(91,95) gas has good air-sensitive performance, therefore has long-range application prospect in formaldehyde gas context of detection.

Description

A kind of preparation method of the Indium sesquioxide. nano-particle with loose structure
Technical field
The present invention relates to the preparation method of a kind of Indium sesquioxide. nano-particle with loose structure, belong to advanced nano functional Material preparation process technical field.
Background technology
In daily life, going on a journey outside, we are endangered by gases such as industrial production waste gas, vehicle exhaust and PM2.5 deeply Evil, is affected by formaldehyde and the toxic gas such as stupid again in interior house.Therefore, either for environmental pollution gas detecting It is badly in need of, or to ensureing quality of life and the serious hope of industrial safety, researches and develops high performance gas sensor and possess very Important realistic meaning.Along with people are to the pay attention to day by day of environmental issue and the strict monitoring to toxic and harmful discharge, respectively Gas examination and the prior-warning device of planting Various Functions are raw therewith, and have obtained industrialization and commercialization further.Owing to partly leading Bromhidrosis body sensor has detection sensitivity height, response recovers fast, circuit is simple, simple to operate, component size is less, price is low The feature such as honest and clean, is widely used in various field of gas detection.
In2O3Having bigger energy gap, band gap, close to GaN, has low-resistivity, Gao Ling in visible region The advantages such as sensitivity, low operating temperature, low absorptance and high infrared reflection rate.Affect In2O3The principal element of nano ZnO is Its structure and morphology, the most currently, a lot of research worker are devoted to control In2O3The research that crystal morphology generates, in order to improve with this The performance of its each side.In recent years, European and American developed countries report answering in optoelectronic film field indium oxide nanometer material in succession With.At present, research worker by vapor phase method, solid phase method, the nano material synthetic method of liquid phase method prepared one-dimensional, two-dimentional, Three-dimensional In2O3Nano material.Its concrete pattern has nanotube, nano wire, nanometer rods, cube and octahedron etc., is widely used In fields such as optics, magnetics, electronics, medical treatment.In order to improve identification function, except selecting good matrix material, by adulterating, Compound and surface is modified outside being modified, and designs and prepares and has bigger serface, the porous of high activity site density and grade Level structure material is also affected by the strategy paid close attention to.The Indium sesquioxide. that the present invention prepares has loose structure, has good penetrating Property, it is possible to promote gas diffusion, the beneficially raising of sensitive body utilization rate.Additionally, in order to improve semiconductor gas sensor Sensitivity, people are frequently with the method increasing material surface area, and nanorize is exactly a kind of conventional method.Nanorize is by increasing The surface area of material, makes the height of particle surface potential barrier, with thickness and crystal grain effective resistance, notable change, surface activity occur It is greatly increased, makes the adsorption and desorption of material for gaseous and redox reaction to carry out at lower temperatures, reduce work Make temperature, shorten response time, improve the concentration range of gas detecting.China is for In2O3Nano material especially its knot The research of configuration looks is in the starting stage, but due to shortcomings such as preparation method have operation complexity, and production cost is high, this makes Obtain achievement in research to be difficult to put on a large scale in actual industrial production.Additionally, due to experimental facilities and the restriction of production technology, People are for In at present2O3The probing in terms of especially air-sensitive performance of probing into of nano material is not the most deep.Research worker is urgently Treat with the comprehensive angle of more system to study In2O3The structure and morphology feature of nano material and functional character feature.
Summary of the invention
It is an object of the invention to, overcome the deficiencies in the prior art, it is provided that a kind of Indium sesquioxide. nanometer with loose structure The preparation method of granule.Having low cost, production technology is simple, and productivity is high, non-environmental-pollution, it is easy to industrialization large-scale production Feature.The sensitivity of the Indium sesquioxide. gas sensitive that gained has loose structure is largely increased, and can be used for gas sensor In field.The technical scheme realizing the object of the invention is: the preparation method of a kind of Indium sesquioxide. nano-particle with loose structure, It is characterized in that: with indium chloride and lauryl amine as raw material, through hydro-thermal reaction, calcination processing, obtain the oxidation with loose structure Indium nanometer particle.This method production technology is simple, does not use the surfactant of costliness, and cost ratio is relatively low, and gained Indium sesquioxide. can As gas sensitive, owing to having loose structure.PARA FORMALDEHYDE PRILLS(91,95) gas has good air-sensitive performance, therefore detects at formaldehyde gas Aspect has long-range application prospect.Concrete synthesis step is as follows:
(1) weighing a certain amount of indium chloride, lauryl amine, be dissolved in dehydrated alcohol, wherein the concentration of indium chloride is 0.02-0.05 Mol/L, the concentration of lauryl amine is 0.02-0.05 mol/L, and the mol ratio controlling indium chloride and lauryl amine is 1:(1-2);
(2) by during in step (1), gained mixed solution moves to the hydrothermal reaction kettle that liner is politef, at 170-200 DEG C At a temperature of, carry out hydro-thermal reaction 8-20 hour, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and spend Gained solid product is repeatedly washed by ionized water and ethanol;
(3) being positioned in drying baker by step (2) gained solid product, 60 DEG C are dried 24 hours, are subsequently placed in alumina crucible Put into Muffle furnace, heat treatment 3 hours at 400-550 DEG C, obtain the Indium sesquioxide. powder body with loose structure.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the Indium sesquioxide. nano-particle with loose structure.
Fig. 2 is the SEM figure of the Indium sesquioxide. nano-particle with loose structure.
Fig. 3 is the TEM figure of the Indium sesquioxide. nano-particle with loose structure.
Fig. 4 is the HRTEM figure of the Indium sesquioxide. nano-particle with loose structure.
Fig. 5 is the formaldehyde gas to 10-500ppm of the Indium sesquioxide. gas sensor under optimum operating voltage with loose structure Sensitivity curve figure.
Fig. 6 is the response recovery curve figure of the Indium sesquioxide. gas sensor under optimum operating voltage with loose structure.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is carried out under premised on technical solution of the present invention Implement, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following enforcement Example.
Embodiment 1
(1) weighing a certain amount of indium chloride, lauryl amine, be dissolved in dehydrated alcohol, wherein the concentration of indium chloride is 0.025 mol/ L, the concentration of lauryl amine is 0.025 mol/L, and the mol ratio controlling indium chloride and lauryl amine is 1:1;
(2) by during in step (1), gained mixed solution moves to the hydrothermal reaction kettle that liner is politef, 170 DEG C of temperature Under, carry out hydro-thermal reaction 8 hours, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and use deionized water With ethanol, gained solid product is repeatedly washed;
(3) being positioned in drying baker by step (2) gained solid product, 60 DEG C are dried 24 hours, are subsequently placed in alumina crucible Put into Muffle furnace, heat treatment 3 hours at 400 DEG C, obtain the Indium sesquioxide. powder body with loose structure.
Embodiment 2
(1) weighing a certain amount of indium chloride, lauryl amine, be dissolved in dehydrated alcohol, wherein the concentration of indium chloride is 0.028 mol/ L, the concentration of lauryl amine is 0.028 mol/L, and the mol ratio controlling indium chloride and lauryl amine is 1:1;
(2) by during in step (1), gained mixed solution moves to the hydrothermal reaction kettle that liner is politef, 180 DEG C of temperature Under, carry out hydro-thermal reaction 12 hours, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and use deionized water With ethanol, gained solid product is repeatedly washed;
(3) being positioned in drying baker by step (2) gained solid product, 60 DEG C are dried 24 hours, are subsequently placed in alumina crucible Put into Muffle furnace, heat treatment 3 hours at 400 DEG C, obtain the Indium sesquioxide. powder body with loose structure.
Embodiment 3
(1) weighing a certain amount of indium chloride, lauryl amine, be dissolved in dehydrated alcohol, wherein the concentration of indium chloride is 0.028 mol/ L, the concentration of lauryl amine is 0.056 mol/L, and the mol ratio controlling indium chloride and lauryl amine is 1:2;
(2) by during in step (1), gained mixed solution moves to the hydrothermal reaction kettle that liner is politef, 180 DEG C of temperature Under, carry out hydro-thermal reaction 12 hours, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and use deionized water With ethanol, gained solid product is repeatedly washed;
(3) being positioned in drying baker by step (2) gained solid product, 60 DEG C are dried 24 hours, are subsequently placed in alumina crucible Put into Muffle furnace, heat treatment 3 hours at 400 DEG C, obtain the Indium sesquioxide. powder body with loose structure.
Embodiment 4
(1) weighing a certain amount of indium chloride, lauryl amine, be dissolved in dehydrated alcohol, wherein the concentration of indium chloride is 0.028 mol/ L, the concentration of lauryl amine is 0.028 mol/L, and the mol ratio controlling indium chloride and lauryl amine is 1:1;
(2) by during in step (1), gained mixed solution moves to the hydrothermal reaction kettle that liner is politef, 200 DEG C of temperature Under, carry out hydro-thermal reaction 16 hours, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and use deionized water With ethanol, gained solid product is repeatedly washed;
(3) being positioned in drying baker by step (2) gained solid product, 60 DEG C are dried 24 hours, are subsequently placed in alumina crucible Put into Muffle furnace, heat treatment 3 hours at 400 DEG C, obtain the Indium sesquioxide. powder body with loose structure.
Embodiment 5
(1) weighing a certain amount of indium chloride, lauryl amine, be dissolved in dehydrated alcohol, wherein the concentration of indium chloride is 0.028 mol/ L, the concentration of lauryl amine is 0.028 mol/L, and the mol ratio controlling indium chloride and lauryl amine is 1:1;
(2) by during in step (1), gained mixed solution moves to the hydrothermal reaction kettle that liner is politef, 200 DEG C of temperature Under, carry out hydro-thermal reaction 20 hours, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and use deionized water With ethanol, gained solid product is repeatedly washed;
(3) being positioned in drying baker by step (2) gained solid product, 60 DEG C are dried 24 hours, are subsequently placed in alumina crucible Put into Muffle furnace, heat treatment 3 hours at 400 DEG C, obtain the Indium sesquioxide. powder body with loose structure.

Claims (1)

1. having a preparation method for the Indium sesquioxide. nano-particle of loose structure, concrete synthesis step is as follows:
(1) weighing a certain amount of indium chloride, lauryl amine, be dissolved in dehydrated alcohol, wherein the concentration of indium chloride is 0.02-0.05 Mol/L, the concentration of lauryl amine is 0.02-0.05 mol/L, and the mol ratio controlling indium chloride and lauryl amine is 1:(1-2);
(2) by during in step (1), gained mixed solution moves to the hydrothermal reaction kettle that liner is politef, at 170-200 DEG C At a temperature of, carry out hydro-thermal reaction 8-20 hour, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and spend Gained solid product is repeatedly washed by ionized water and ethanol;
(3) being positioned in drying baker by step (2) gained solid product, 60 DEG C are dried 24 hours, are subsequently placed in alumina crucible Put into Muffle furnace, heat treatment 3 hours at 400-550 DEG C, obtain the Indium sesquioxide. powder body with loose structure.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107024518A (en) * 2017-04-18 2017-08-08 中国工程物理研究院化工材料研究所 Three-dimensional structure nano indium oxide gas sensor and preparation method thereof
CN107032389A (en) * 2017-06-16 2017-08-11 宁波大学 A kind of porous oxidation indium nano material and preparation method thereof
CN107215889A (en) * 2017-06-28 2017-09-29 济南大学 A kind of preparation method of loose structure indium oxide cube gas sensitive
CN107285392A (en) * 2017-06-28 2017-10-24 济南大学 A kind of NiO In2O3The preparation method of nano composite material
CN107381622A (en) * 2017-06-28 2017-11-24 济南大学 A kind of rGO In2O3The preparation method of nanoparticle composite
CN110871077A (en) * 2019-11-09 2020-03-10 上海纳米技术及应用国家工程研究中心有限公司 Preparation of gamma-aluminum oxide In-loaded cobaltosic oxide material with high-temperature stability, product and application

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CN101182031A (en) * 2007-11-27 2008-05-21 山东大学 Method for preparing indium oxide nano thread ordered aggregation

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107024518A (en) * 2017-04-18 2017-08-08 中国工程物理研究院化工材料研究所 Three-dimensional structure nano indium oxide gas sensor and preparation method thereof
CN107032389A (en) * 2017-06-16 2017-08-11 宁波大学 A kind of porous oxidation indium nano material and preparation method thereof
CN107032389B (en) * 2017-06-16 2018-07-03 宁波大学 A kind of porous oxidation indium nano material and preparation method thereof
CN107215889A (en) * 2017-06-28 2017-09-29 济南大学 A kind of preparation method of loose structure indium oxide cube gas sensitive
CN107285392A (en) * 2017-06-28 2017-10-24 济南大学 A kind of NiO In2O3The preparation method of nano composite material
CN107381622A (en) * 2017-06-28 2017-11-24 济南大学 A kind of rGO In2O3The preparation method of nanoparticle composite
CN110871077A (en) * 2019-11-09 2020-03-10 上海纳米技术及应用国家工程研究中心有限公司 Preparation of gamma-aluminum oxide In-loaded cobaltosic oxide material with high-temperature stability, product and application
CN110871077B (en) * 2019-11-09 2022-11-01 上海纳米技术及应用国家工程研究中心有限公司 Preparation of gamma-aluminum oxide In-loaded cobaltosic oxide material with high-temperature stability, product and application

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