CN107285392A - A kind of NiO In2O3The preparation method of nano composite material - Google Patents

A kind of NiO In2O3The preparation method of nano composite material Download PDF

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CN107285392A
CN107285392A CN201710504939.5A CN201710504939A CN107285392A CN 107285392 A CN107285392 A CN 107285392A CN 201710504939 A CN201710504939 A CN 201710504939A CN 107285392 A CN107285392 A CN 107285392A
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张苏
宋鹏
王�琦
杨中喜
田哲宾
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Abstract

The invention provides a kind of NiO In2O3The preparation method of nano composite material.The preparation method is specifically included：With four trichloride hydrate indiums, lauryl amine is raw material, through hydro-thermal reaction, and indium oxide nanoparticle is obtained after calcination processing；And then with Nickelous nitrate hexahydrate, hexamethylenetetramine and trisodium citrate are raw material, in the nickel oxide of indium oxide microsphere surface compound sheet, finally give NiO In2O3Nano composite material.This method simple production process, gained gas sensitive has the p n hetero-junctions that indium oxide is constituted with nickel oxide, it shows higher sensitivity and quickly response, recovery to acetone, available for acetone gas sensor field, so as to obtain highly sensitive new gas sensitive.

Description

A kind of NiO-In2O3The preparation method of nano composite material
Technical field
The present invention relates to a kind of NiO-In2O3The preparation method of nano composite material, belongs to advanced nano-functional material and prepares Technology field.
Background technology
With the aggravation of environmental pollution, the qualitative and quantitative detection for toxic and harmful gas seems more and more important.It is existing Nowadays, what the analysis to these gases was generally used is all that time-consuming and expensive tester, such as spectrum for some tests Analysis, chromatography.Due to metal oxide semiconductor gas sensor have high sensitivity, high selectivity, quick response and Cheap the advantages of, therefore future can be the ideal of detection toxic and harmful gas, and have the replacement of application prospect Product.In these metal oxide semiconductors, In2O3It is a kind of new gas sensitive, with SnO2、ZnO、Fe2O3Deng traditional gas Quick material is compared, and it has the advantages that wider energy gap, less resistivity and higher catalytic activity.Although single group The potentiality of the application prospect of the gas sensor of the indium oxide nanostructure divided, but still there is selectivity in actual applications Difference, the shortcomings of operating temperature is high.In order to improve the air-sensitive performance of indium oxide, control micro/nano structure functional material pattern and Structure is to influence the principal element of its application performance, and many people have been directed to control the pattern and knot of material in preparation process Structure either develops new construction to realize the enhancing of performance.
For the air-sensitive performance of material, we can make to form heterogeneous between different band gap and the semi-conducting material of energy level Junction structure.Heterojunction structure is built while material morphology is controlled, will be improved air-sensitive performance.However, such a The method of important raising material air-sensitive performance does not obtain sufficient investigation and research also.Nickel oxide is a kind of good p types Semiconductor, it is widely used in terms of catalyst, electrode, biology sensor and magnetic material.In recent years, also someone studies On the problem of NiO hetero-junctions, such as Shouli Bai（Shouli Bai, Jingchao Liu, Jun Guo, Ruixian Luo, Facile preparation of SnO2/NiO composites and enhancement of sensing performance to NO2, Sensors and Actuators B 249 (2017) 22-29）It is prepared for tin oxide and oxygen Change the nano composite material of nickel, and composite has obtained significantly increasing for the air-sensitive performance of nitrogen dioxide.Thus As can be seen that the gas sensitive that design and the indium oxide of synthesis are combined with nickel oxide is by with important science and practice significance. However, as far as we know, it is also seldom that the gas sensitive that indium oxide is combined with nickel oxide is reported.Therefore during this investigation it turned out, We prepare indium oxide nanoparticle and heterogeneous with the nickel oxide modification indium oxide nanoparticle formation p-n of sheet by hydro-thermal method Junction structure has simultaneously carried out system research to its microstructure and air-sensitive performance.
The content of the invention
It is an object of the present invention to overcome the deficiencies in the prior art, there is provided a kind of NiO-In2O3The system of nano composite material Preparation Method.Low with cost, simple production process, yield is high, the characteristics of non-environmental-pollution.Gained indium oxide is combined with nickel oxide The sensitivity of gas sensitive obtain a certain degree of raising compared to pure zirconia indium oxide, led available for gas sensor etc. Domain.Realizing the technical scheme of the object of the invention is：A kind of NiO-In2O3The preparation method of nano composite material, it is characterised in that： With four trichloride hydrate indiums, lauryl amine is raw material, through hydro-thermal reaction, and indium oxide nanoparticle is obtained after calcination processing；And then with Nickelous nitrate hexahydrate, hexamethylenetetramine and trisodium citrate are raw material, in the oxidation of indium oxide microsphere surface compound sheet Nickel, finally gives NiO-In2O3Nano composite material.This method simple production process, gained gas sensitive has indium oxide and oxygen Change the p-n heterojunction that nickel is constituted, it shows higher sensitivity to acetone and quickly responds, recovers, available for acetone gas Body sensor field, so as to obtain highly sensitive new gas sensitive.Specific synthesis step is as follows：
（1）A certain amount of four trichloride hydrates indium, lauryl amine are weighed, is dissolved in 35 mL absolute ethyl alcohols, wherein four trichloride hydrates The concentration of indium is 0.02-0.05 mol/L, and the concentration of lauryl amine is 0.02-0.05 mol/L, and controls four trichloride hydrate indiums Mol ratio with lauryl amine is 1:(1-2)；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180-200 DEG C At a temperature of, carry out hydro-thermal reaction 8-16 h, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and spend from Sub- water and ethanol are repeatedly washed to gained solid product, and gained solid product is positioned in drying box, 60 DEG C of dryings, It is subsequently placed in alumina crucible and is put into Muffle furnace, 3 h are heat-treated at 400-550 DEG C, obtains indium oxide powder；
（3）By step（2）The indium oxide powder of gained is scattered in 40 mL deionized waters, weighs a certain amount of six nitric hydrate Nickel, hexamethylenetetramine and trisodium citrate are dissolved in above-mentioned solution, and are stirred.Mixed solution is placed in 60-90 6 h are incubated in DEG C water-bath, reaction dries washing of precipitate after terminating.Wherein the concentration of Nickelous nitrate hexahydrate is 0.01-0.03 Mol/L, the concentration of hexamethylenetetramine is 0.01-0.03 mol/L, and the concentration of trisodium citrate is 0.001-0.003 mol/ L, and the mol ratio of Nickelous nitrate hexahydrate and indium oxide is controlled for (3-5):1, control Nickelous nitrate hexahydrate and hexamethylenetetramine Mol ratio be 1:(1-2), the mol ratio for controlling Nickelous nitrate hexahydrate and trisodium citrate is (5-10):1；
（4）By step（3）Gained solid product is heat-treated 2 h at 400-500 DEG C, you can obtain NiO-In2O3It is nano combined Material.
Brief description of the drawings
Fig. 1 is NiO-In2O3The XRD spectrum of nano composite material.
Fig. 2 is NiO-In2O3The FESEM figures of nano composite material.
Fig. 3 is NiO-In2O3The EDS collection of illustrative plates of nano composite material.
Fig. 4 is NiO-In2O3The TEM figures of nano composite material.
Fig. 5 is NiO-In under optimum operating voltage2O3Nano composite material gas sensor and pure zirconia indium gas sensor pair The sensitivity curve comparison diagram of 20-1000ppm front three amine gas.
Fig. 6 is NiO-In under optimum operating voltage2O3The sound of nano composite material gas sensor and pure zirconia indium gas sensor Recovery curve is answered to contrast.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations Example.
Embodiment 1
（1）A certain amount of four trichloride hydrates indium, lauryl amine are weighed, is dissolved in 35 mL absolute ethyl alcohols, wherein four trichloride hydrates The concentration of indium is 0.025 mol/L, and the concentration of lauryl amine is 0.025 mol/L, and controls four trichloride hydrate indiums and lauryl amine Mol ratio be 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 180 DEG C of temperature Under, carry out the h of hydro-thermal reaction 8, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with Ethanol is repeatedly washed to gained solid product, and gained solid product is positioned in drying box, 60 DEG C of dryings, is then put Muffle furnace is put into alumina crucible, 3 h are heat-treated at 500 DEG C, indium oxide powder is obtained；
（3）By step（2）The indium oxide powder of gained is scattered in 40 mL deionized waters, weighs a certain amount of six nitric hydrate Nickel, hexamethylenetetramine and trisodium citrate are dissolved in above-mentioned solution, and are stirred.Mixed solution is placed in 60 DEG C 6 h are incubated in water-bath, reaction dries washing of precipitate after terminating.Wherein the concentration of Nickelous nitrate hexahydrate is 0.015 mol/L, six The concentration of methine tetramine is 0.015 mol/L, and the concentration of trisodium citrate is 0.0015 mol/L, and controls six nitric hydrates The mol ratio of nickel and indium oxide is 3:1, the mol ratio for controlling Nickelous nitrate hexahydrate and hexamethylenetetramine is 1:1, control six water The mol ratio for closing nickel nitrate and trisodium citrate is 10:1；
（4）By step（3）Gained solid product is heat-treated 2 h at 400 DEG C, you can obtain NiO-In2O3Nano combined material Material.
Embodiment 2
（1）A certain amount of four trichloride hydrates indium, lauryl amine are weighed, is dissolved in 35 mL absolute ethyl alcohols, wherein four trichloride hydrates The concentration of indium is 0.025 mol/L, and the concentration of lauryl amine is 0.025 mol/L, and controls four trichloride hydrate indiums and lauryl amine Mol ratio be 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 180 DEG C of temperature Under, carry out the h of hydro-thermal reaction 12, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with Ethanol is repeatedly washed to gained solid product, and gained solid product is positioned in drying box, 60 DEG C of dryings, is then put Muffle furnace is put into alumina crucible, 3 h are heat-treated at 500 DEG C, indium oxide powder is obtained；
（3）By step（2）The indium oxide powder of gained is scattered in 40 mL deionized waters, weighs a certain amount of six nitric hydrate Nickel, hexamethylenetetramine and trisodium citrate are dissolved in above-mentioned solution, and are stirred.Mixed solution is placed in 90 DEG C 6 h are incubated in water-bath, reaction dries washing of precipitate after terminating.Wherein the concentration of Nickelous nitrate hexahydrate is 0.015 mol/L, six The concentration of methine tetramine is 0.015 mol/L, and the concentration of trisodium citrate is 0.0015 mol/L, and controls six nitric hydrates The mol ratio of nickel and indium oxide is 3:1, the mol ratio for controlling Nickelous nitrate hexahydrate and hexamethylenetetramine is 1:1, control six water The mol ratio for closing nickel nitrate and trisodium citrate is 10:1；
（4）By step（3）Gained solid product is heat-treated 2 h at 400 DEG C, you can obtain NiO-In2O3Nano combined material Material.
Embodiment 3
（1）A certain amount of four trichloride hydrates indium, lauryl amine are weighed, is dissolved in 35 mL absolute ethyl alcohols, wherein four trichloride hydrates The concentration of indium is 0.025 mol/L, and the concentration of lauryl amine is 0.05 mol/L, and four trichloride hydrate indiums of control and lauryl amine Mol ratio is 1:2；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 200 DEG C of temperature Under, carry out the h of hydro-thermal reaction 16, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with Ethanol is repeatedly washed to gained solid product, and gained solid product is positioned in drying box, 60 DEG C of dryings, is then put Muffle furnace is put into alumina crucible, 3 h are heat-treated at 500 DEG C, indium oxide powder is obtained；
（3）By step（2）The indium oxide powder of gained is scattered in 40 mL deionized waters, weighs a certain amount of six nitric hydrate Nickel, hexamethylenetetramine and trisodium citrate are dissolved in above-mentioned solution, and are stirred.Mixed solution is placed in 90 DEG C 6 h are incubated in water-bath, reaction dries washing of precipitate after terminating.Wherein the concentration of Nickelous nitrate hexahydrate is 0.015 mol/L, six The concentration of methine tetramine is 0.03 mol/L, and the concentration of trisodium citrate is 0.0015 mol/L, and controls six nitric hydrates The mol ratio of nickel and indium oxide is 3:1, the mol ratio for controlling Nickelous nitrate hexahydrate and hexamethylenetetramine is 1:2, control six water The mol ratio for closing nickel nitrate and trisodium citrate is 10:1；
（4）By step（3）Gained solid product is heat-treated 2 h at 400 DEG C, you can obtain NiO-In2O3Nano combined material Material.
Embodiment 4
（1）A certain amount of four trichloride hydrates indium, lauryl amine are weighed, is dissolved in 35 mL absolute ethyl alcohols, wherein four trichloride hydrates The concentration of indium is 0.025 mol/L, and the concentration of lauryl amine is 0.025 mol/L, and controls four trichloride hydrate indiums and lauryl amine Mol ratio be 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 200 DEG C of temperature Under, carry out the h of hydro-thermal reaction 12, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with Ethanol is repeatedly washed to gained solid product, and gained solid product is positioned in drying box, 60 DEG C of dryings, is then put Muffle furnace is put into alumina crucible, 3 h are heat-treated at 500 DEG C, indium oxide powder is obtained；
（3）By step（2）The indium oxide powder of gained is scattered in 40 mL deionized waters, weighs a certain amount of six nitric hydrate Nickel, hexamethylenetetramine and trisodium citrate are dissolved in above-mentioned solution, and are stirred.Mixed solution is placed in 80 DEG C 6 h are incubated in water-bath, reaction dries washing of precipitate after terminating.Wherein the concentration of Nickelous nitrate hexahydrate is 0.015 mol/L, six The concentration of methine tetramine is 0.015 mol/L, and the concentration of trisodium citrate is 0.003 mol/L, and controls six nitric hydrates The mol ratio of nickel and indium oxide is 3:1, the mol ratio for controlling Nickelous nitrate hexahydrate and hexamethylenetetramine is 1:1, control six water The mol ratio for closing nickel nitrate and trisodium citrate is 5:1；
（4）By step（3）Gained solid product is heat-treated 2 h at 400 DEG C, you can obtain NiO-In2O3Nano combined material Material.
Embodiment 5
（1）A certain amount of four trichloride hydrates indium, lauryl amine are weighed, is dissolved in 35 mL absolute ethyl alcohols, wherein four trichloride hydrates The concentration of indium is 0.025 mol/L, and the concentration of lauryl amine is 0.025 mol/L, and controls four trichloride hydrate indiums and lauryl amine Mol ratio be 1:1；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 200 DEG C of temperature Under, carry out the h of hydro-thermal reaction 8, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with Ethanol is repeatedly washed to gained solid product, and gained solid product is positioned in drying box, 60 DEG C of dryings, is then put Muffle furnace is put into alumina crucible, 3 h are heat-treated at 500 DEG C, indium oxide powder is obtained；
（3）By step（2）The indium oxide powder of gained is scattered in 40 mL deionized waters, weighs a certain amount of six nitric hydrate Nickel, hexamethylenetetramine and trisodium citrate are dissolved in above-mentioned solution, and are stirred.Mixed solution is placed in 90 DEG C 6 h are incubated in water-bath, reaction dries washing of precipitate after terminating.Wherein the concentration of Nickelous nitrate hexahydrate is 0.015 mol/L, six The concentration of methine tetramine is 0.03 mol/L, and the concentration of trisodium citrate is 0.003 mol/L, and controls Nickelous nitrate hexahydrate Mol ratio with indium oxide is 3:1, the mol ratio for controlling Nickelous nitrate hexahydrate and hexamethylenetetramine is 1:2, control six is hydrated The mol ratio of nickel nitrate and trisodium citrate is 5:1；
（4）Gained solid product is heat-treated 2 h at 400 DEG C, you can obtain NiO-In2O3Nano composite material.

Claims (1)

1. a kind of NiO-In2O3The preparation method of nano composite material, specific synthesis step is as follows：
（1）A certain amount of four trichloride hydrates indium, lauryl amine are weighed, is dissolved in 35 mL absolute ethyl alcohols, wherein four trichloride hydrates The concentration of indium is 0.02-0.05 mol/L, and the concentration of lauryl amine is 0.02-0.05 mol/L, and controls four trichloride hydrate indiums Mol ratio with lauryl amine is 1:(1-2)；
（2）By step（1）Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180-200 DEG C At a temperature of, carry out hydro-thermal reaction 8-16 h, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and spend from Sub- water and ethanol are repeatedly washed to gained solid product, and gained solid product is positioned in drying box, 60 DEG C of dryings, It is subsequently placed in alumina crucible and is put into Muffle furnace, 3 h are heat-treated at 400-550 DEG C, obtains indium oxide powder；
（3）By step（2）The indium oxide powder of gained is scattered in 40 mL deionized waters, weighs a certain amount of six nitric hydrate Nickel, hexamethylenetetramine and trisodium citrate are dissolved in above-mentioned solution, and are stirred, and mixed solution is placed in into 60-90 6 h are incubated in DEG C water-bath, reaction dries washing of precipitate after terminating, wherein the concentration of Nickelous nitrate hexahydrate is 0.01-0.03 Mol/L, the concentration of hexamethylenetetramine is 0.01-0.03 mol/L, and the concentration of trisodium citrate is 0.001-0.003 mol/ L, and the mol ratio of Nickelous nitrate hexahydrate and indium oxide is controlled for (3-5):1, control Nickelous nitrate hexahydrate and hexamethylenetetramine Mol ratio be 1:(1-2), the mol ratio for controlling Nickelous nitrate hexahydrate and trisodium citrate is (5-10):1；
（4）By step（3）Gained solid product is heat-treated 2 h at 400-500 DEG C, you can obtain NiO-In2O3It is nano combined Material.
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Cited By (7)

* Cited by examiner, † Cited by third party
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CN108132282A (en) * 2017-12-20 2018-06-08 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of continuous two-sided hetero-junctions sandwich and products thereof and application
CN109019673A (en) * 2018-08-01 2018-12-18 济南大学 A kind of SnO2-In2O3The preparation method of nanocomposite
CN109052496A (en) * 2018-08-01 2018-12-21 济南大学 A kind of RuO2-In2O3The preparation method of nanocomposite
CN109205686A (en) * 2018-11-21 2019-01-15 上海纳米技术及应用国家工程研究中心有限公司 Nickel oxide based on MOF/indium sesquioxide heterojunction nanometer material preparation method and product and application
CN109632893A (en) * 2019-01-11 2019-04-16 东北大学 One kind being based on p-n heterojunction structure NiO-In2O3The gas sensor of composite Nano ball
CN110280276A (en) * 2019-07-08 2019-09-27 福州大学 Loaded photocatalyst NiSe2The preparation method and applications of/CdS
CN111097420A (en) * 2018-10-26 2020-05-05 中国科学院过程工程研究所 Nickel-based ozonolysis catalyst and preparation method and application thereof

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