CN105753051A - Au nano particle/MoO3 nanorod heterojunction material with trimethylamine sensitizing effect - Google Patents

Au nano particle/MoO3 nanorod heterojunction material with trimethylamine sensitizing effect Download PDF

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CN105753051A
CN105753051A CN201610069118.9A CN201610069118A CN105753051A CN 105753051 A CN105753051 A CN 105753051A CN 201610069118 A CN201610069118 A CN 201610069118A CN 105753051 A CN105753051 A CN 105753051A
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moo3
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moo
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张佳
闫慧慧
宋鹏
王�琦
杨中喜
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
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    • C01—INORGANIC CHEMISTRY
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
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    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
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Abstract

The invention provides a preparation method of an Au nano particle/MoO3 nanorod heterojunction material and relates to the field of production of nano materials. The method comprises the following steps: sintering ammonium paramolybdate to obtain MoO3 powder; mixing and stirring a certain amount of molybdenum oxide powder and H2O2, then adding concentrated nitric acid and distilled water, washing and then drying to obtain rod-like MoO3; dispersing the rod-like MoO3 into deionized water, adding a certain amount of HAuCl4 and L-lysine, stirring, and then adding a certain amount of sodium citrate; heating the obtained solution, centrifugalizing, washing and drying, thereby obtaining the Au nano particle/MoO3 nano material. The preparation method of the Au nano particle/MoO3 nanorod heterojunction material is simple in process, low in equipment requirement, high in operability, relatively low in cost and capable of realizing large-batch synthesis; the obtained nano material has relatively large surface area and relatively small grain size, is low in clustering possibility, has wide application prospect and has a favorable gas-sensitive property on a trimethylamine gas.

Description

A kind of Au nano-particle/MoO with trimethylamine sensitlzing effect3Nanorod heterojunction Material
Technical field
The present invention relates to the production field of nano material, specifically a kind of Au nano-particle/MoO3Nanometer rods is heterogeneous The preparation method of knot material.
Background technology
MoO3Transition metal oxide, is a kind of important broad-band gap (3.2eV) n-type semiconductor functional material, and it is unique Layer structure make it have potential at battery material, catalyst and sensing element etc. and be widely applied.As gas sensitive MoO3Nano material has the features such as high specific surface area, electronic energy transmission vertically, but is used alone MoO3Nano material passes Its selectivity of the material of sensor and sensitivity are the best, and therefore we need to improve it, improve now gas sensitive Method be concentrated mainly on nano composite metal oxide, adulterate or the approach such as load.Trimethylamine gas is had by the present invention Well gas sensing property, trimethylamine belongs to vaporous pollutant, for the colourless gas having fish oil smelly under room temperature, inflammable and explosive, and to people Body eye, nose, throat and respiratory tract have intense stimulus effect, and Long Term Contact harm is relatively big, therefore limit concentration the standard of trimethylamine Really measure significant.
Preparation method about Au support materials has had relevant report at present.(the Feng-such as Feng-Chao Chung Chao Chung, Zhen Zhu, Peng-Yi Luo, Ren-Jang Wu, Wei Li. Au@ZnO core–shell structure for gaseous formaldehyde sensing at room temperature [J]. Sensors And Actuators B 199 (2014) 314-319), prepare with tetra chlorauric acid, zinc sulfate and trisodium citrate etc. for raw material Sensitivity and the selectivity of the Au@ZnO Core-shell structure material PARA FORMALDEHYDE PRILLS(91,95) gas gone out are significantly improved；Hyeon-Min Song etc. (Hyeon-Min Song, Bum-Soo Chon, Seung-Ho Jeon, Prabhakar Rai, Yeon-Tae Yu, Prabir K. Dutta. Synthesis of Au@SnO2 core-shell nanoparticles with controllable shell thickness and their CO sensing properties [J]. Materials Chemistry and Physics 166 (2015) 87-94), with tetra chlorauric acid, sodium hydroxide and sodium stannate etc. as raw material, adopt Au SnO has been synthesized by microwave-assisted hydro-thermal method2Core-shell nano, this material has preferable sensitivity to CO.Above-mentioned side Legal system Preparation Method is complicated, is difficult to operation, and efficiency is low, and the stability being fabricated to device is bad, is not suitable for producing.Also do not have at present It is related to Au@MoO3The relevant report of the preparation method of nano material, and raw material of the present invention is easy to get, low cost and prepared receiving Rice material is difficult to reunite, and has the value of research.
Summary of the invention
A kind of Au nano-particle of offer is provided and is supported on MoO3Preparation method in nanometer rods, the letter of the method technique Single, equipment requirements is low, workable, and cost ratio is relatively low, and can synthesize in a large number, and the nano material obtained has bigger table Area and less crystallite dimension, be difficult to reunite, have a wide range of applications future.
The present invention is realized by following technical method: ammonium paramolybdate calcining is obtained MoO3Powder；By a certain amount of oxygen Change molybdenum powder and H2O2Stir after mixing, add concentrated nitric acid and distilled water, through washing and obtaining bar-shaped MoO after drying3；Will A certain amount of bar-shaped MoO3It is distributed in deionized water, after solution mixes, adds the acid of a certain amount of tetrachloro alloy and L- Lysine, and stir and make mix homogeneously, then toward above-mentioned mixed solution is added dropwise over a certain amount of sodium citrate, by centrifugation, Washing, be dried, then be placed in Muffle furnace calcining obtain Au nano-particle/MoO3Nano material.Specifically comprise the following steps that
(1) a certain amount of ammonium paramolybdate (AHM) is calcined at 500 DEG C within four hours, obtain MoO3Powder；
(2) a certain amount of MoO is taken3Powder is dissolved in the H of 30%2O2In, stir 4-8 hour, wherein the amount of molybdenum oxide powder is 1.6-7.2g, H2O2Amount be 12.2-55ml；
(3) a certain amount of concentrated nitric acid and distilled water are added in step (2), obtain transparent yellow peroxo-polymolybdic acid solution；Wherein The amount of concentrated nitric acid is 6-27ml, and the amount of distilled water is 42.2-170ml；
(4) solution that step (3) obtains is moved in the hydrothermal reaction kettle that liner is politef, anti-at 150-220 DEG C Answer 40-50 hour, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol to institute Obtain solid product repeatedly to wash；
(5) product that step (4) obtains is placed in drying baker, is dried 24 hours at 60 DEG C, obtains one-dimensional bar-shaped molybdenum oxide；
(6) weighing a certain amount of bar-shaped molybdenum oxide to be distributed in 15ml deionized water, wherein the amount of molybdenum oxide is 0.02-0.1g；
(7) adding the acid of 1ml tetrachloro alloy and 1B in step (6), wherein the concentration of 1B is that 0.01-0.1 rubs You/liter；
(8) in the solution that step (7) mixes, it is added dropwise over a certain amount of sodium citrate, stirs 30-60 minute；Wherein Fructus Citri Limoniae Acid na concn is 0.1-0.2 mol/L；
(9) by the solution of gained in step (8), centrifuge is utilized to carry out solid-liquid separation, and with deionized water and ethanol to gained Solid product repeatedly washs, and is dried 24 hours, is subsequently placed in alumina crucible and puts into Muffle furnace in drying baker at 60 DEG C, Calcine 30-60 minute at 300-400 DEG C.
Au nano-particle/MoO that the present invention succeeds in developing3Nanorod heterojunction material, this material is in the sensitivity of gas All increase with on selectivity, and for Au nano-particle/MoO3The research of nanorod heterojunction material there is not yet report Road.This nano material has bigger surface area and less crystallite dimension, is difficult to reunite, and with low cost, easy to operate, Have a wide range of applications future.
Accompanying drawing illustrates:
Fig. 1 is bar-shaped MoO in embodiment 13The FESEM picture of nano material；
Fig. 2 is Au nano-particle/MoO in embodiment 13The FESEM picture of nanorod heterojunction material；
Fig. 3 is Au nano-particle/MoO in embodiment 13The X ray diffracting spectrum of nanorod heterojunction material；
Fig. 4 is Au nano-particle/MoO in embodiment 13The transmission electron microscope TEM collection of illustrative plates of nanorod heterojunction material；
Fig. 5 is Au nano-particle/MoO in embodiment 13The transmission electron microscope TEM collection of illustrative plates of nanorod heterojunction material；
Fig. 6 is MoO in embodiment 13With Au nano-particle/MoO3Nanorod heterojunction material is at the working temperature to variable concentrations The response curve of trimethylamine gas.
Detailed description of the invention
Embodiment 1
(1) a certain amount of ammonium paramolybdate (AHM) is calcined at 500 DEG C within four hours, obtain MoO3Powder；
(2) a certain amount of MoO is taken3Powder is dissolved in the H of 30%2O2In, stir 6 hours, wherein the amount of molybdenum oxide powder is 7.2g, H2O2Amount be 55ml；
(3) a certain amount of concentrated nitric acid and distilled water are added in step (2), obtain transparent yellow peroxo-polymolybdic acid solution；Wherein The amount of concentrated nitric acid is 27ml, and the amount of distilled water is 170ml；
(4) solution that step (3) obtains is moved in the hydrothermal reaction kettle that liner is politef, at 170 DEG C, react 45 Hour, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol to gained solid Product repeatedly washs；
(5) product that step (4) obtains is placed in drying baker, is dried 24 hours at 60 DEG C, obtains one-dimensional bar-shaped molybdenum oxide；
(6) weigh a certain amount of molybdenum oxide to be distributed in 15ml deionized water, wherein amount 0.05g of molybdenum oxide；
(7) adding the acid of 1ml tetrachloro alloy and 1B in step (6) and stir, wherein 1B concentration is 0.01 Mol/L；
(8) in the solution that step (7) mixes, it is added dropwise over sodium citrate, stirs 30 minutes, the wherein concentration of sodium citrate It it is 0.1 mol/L；
(9) solution of step (8) gained utilize centrifuge carry out solid-liquid separation, and with deionized water and ethanol to gained solid Product repeatedly washs, and is dried 24 hours, is subsequently placed in alumina crucible and puts into Muffle furnace in drying baker at 60 DEG C, At 300 DEG C, calcining obtains Au nano-particle/MoO for 30 minutes3Nanorod heterojunction material.
The bar-shaped MoO prepared by embodiment 13The FESEM collection of illustrative plates of nano material is as shown in Figure 1, it can be seen that prepare Sample topography is complete；Au nano-particle/MoO3The FESEM collection of illustrative plates of nano material is as shown in fig. 2, it can be seen that Au is with nanometer The form of grain is supported on MoO3In nanometer rods, and Au nano-particle is less and distribution ratio is more uniform.
Au nano-particle/the MoO prepared by embodiment 13The X ray diffracting spectrum of nanorod heterojunction material such as Fig. 3 Shown in, the position of all diffraction maximums of the XRD figure spectrum of employing sample prepared by the present invention and international standard card PDF#35- 0609, there is no other miscellaneous peak, show that obtained sample comprises only Au and MoO3；The Au nano-particle prepared by embodiment 1/ MoO3The transmission electron microscope TEM of nanorod heterojunction material schemes as shown in Figure 4, and as can be seen from the figure Au nano-particle is smaller, And all at below 10nm.Au nano-particle/the MoO prepared by embodiment 13Nanorod heterojunction material is the most right The response curve of variable concentrations trimethylamine gas is as shown in Figure 6, it can be seen that the trimethylamine of low concentration is responded preferably by this material, And the material of load gold nano grain is than simple MoO3Response to trimethylamine increases.
Embodiment 2
(1) a certain amount of ammonium paramolybdate (AHM) is calcined at 500 DEG C within four hours, obtain MoO3Powder；
(2) a certain amount of MoO is taken3Powder is dissolved in the H of 30%2O2In, stir 6 hours, wherein the amount of molybdenum oxide powder is 2.4g, H2O2Amount be 18.33ml；
(3) a certain amount of concentrated nitric acid and distilled water are added in step (2), obtain transparent yellow peroxo-polymolybdic acid solution；Wherein The amount of concentrated nitric acid is 9ml, and the amount of distilled water is 57.66ml；
(4) solution that step (3) obtains is moved in the hydrothermal reaction kettle that liner is politef, at 170 DEG C, react 45 Hour, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol to gained solid Product repeatedly washs；
(5) product that step (4) obtains is placed in drying baker, is dried 24 hours at 60 DEG C, obtains one-dimensional bar-shaped molybdenum oxide；
(6) weighing a certain amount of molybdenum oxide to be distributed in 15ml deionized water, wherein the amount of molybdenum oxide is 0.05g；
(7) adding the acid of 1ml tetrachloro alloy and 1B in step (6) and stir, wherein 1B concentration is 0.05 Mol/L；
(8) in the solution that step (7) mixes, it is added dropwise over sodium citrate, stirs 50 minutes, the wherein concentration of sodium citrate It it is 0.1 mol/L；
(9) solution of step (8) gained utilize centrifuge carry out solid-liquid separation, and with deionized water and ethanol to gained solid Product repeatedly washs, and is dried 24 hours, is subsequently placed in alumina crucible and puts into Muffle furnace in drying baker at 60 DEG C, At 400 DEG C, calcining obtains Au nano-particle/MoO for 40 minutes3Nanorod heterojunction material.
Embodiment 3
(1) a certain amount of ammonium paramolybdate (AHM) is calcined at 500 DEG C within four hours, obtain MoO3Powder；
(2) a certain amount of MoO is taken3Powder is dissolved in the H of 30%2O2In, stir 6 hours, wherein the amount of molybdenum oxide powder is 7.2g, H2O2Amount be 55ml；
(3) a certain amount of concentrated nitric acid and distilled water are added in step (2), obtain transparent yellow peroxo-polymolybdic acid solution；Wherein The amount of concentrated nitric acid is 27ml, and the amount of distilled water is 170ml；
(4) solution that step (3) obtains is moved in the hydrothermal reaction kettle that liner is politef, at 170 DEG C, react 45 Hour, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol to gained solid Product repeatedly washs；
(5) product that step (4) obtains is placed in drying baker, is dried 24 hours at 60 DEG C, obtains one-dimensional bar-shaped molybdenum oxide；
(6) weighing a certain amount of molybdenum oxide to be distributed in 15ml deionized water, wherein the amount of molybdenum oxide is 0.1g；
(7) adding the acid of 1ml tetrachloro alloy and 1B in step (6) and stir, wherein 1B concentration is 0.02 Mol/L；
(8) in the solution that step (7) mixes, it is added dropwise over sodium citrate, stirs 60 minutes, the wherein concentration of sodium citrate It it is 0.2 mol/L；
(9) solution of step (8) gained utilize centrifuge carry out solid-liquid separation, and with deionized water and ethanol to gained solid Product repeatedly washs, and is dried 24 hours, is subsequently placed in alumina crucible and puts into Muffle furnace in drying baker at 60 DEG C, At 300 DEG C, calcining obtains Au nano-particle/MoO for 40 minutes3Nanorod heterojunction material.

Claims (1)

1. Au nano-particle/MoO with trimethylamine sensitlzing effect3The preparation of nanorod heterojunction material, it is characterised in that There are following steps:
(1) a certain amount of ammonium paramolybdate (AHM) is calcined at 500 DEG C within four hours, obtain MoO3Powder；
(2) a certain amount of MoO is taken3Powder is dissolved in the H of 30%2O2In, stir 4-8 hour, wherein the amount of molybdenum oxide powder is 1.6-7.2g, H2O2Amount be 12.2-55ml；
(3) a certain amount of concentrated nitric acid and distilled water are added in step (2), obtain transparent yellow peroxo-polymolybdic acid solution；Wherein The amount of concentrated nitric acid is 6-27ml, and the amount of distilled water is 42.2-170ml；
(4) solution that step (3) obtains is moved in the hydrothermal reaction kettle that liner is politef, anti-at 150-220 DEG C Answer 40-50 hour, then the product utilization centrifuge after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol to institute Obtain solid product repeatedly to wash；
(5) product that step (4) obtains is placed in drying baker, is dried 24 hours at 60 DEG C, obtains one-dimensional bar-shaped molybdenum oxide；
(6) weighing a certain amount of ribbon molybdenum oxide to be distributed in 15ml deionized water, wherein the amount of molybdenum oxide is 0.02- 0.1g；
(7) adding the acid of 1ml tetrachloro alloy and 1B in step (6) and stir, wherein the concentration of 1B is 0.01-0.1 mol/L；
(8) in the solution that step (7) mixes, it is added dropwise over a certain amount of sodium citrate, stirs 30-60 minute；Wherein Fructus Citri Limoniae Acid na concn is 0.1-0.2 mol/L；
(9) by the solution of gained in step (8), centrifuge is utilized to carry out solid-liquid separation, and with deionized water and ethanol to gained Solid product repeatedly washs, and is dried 24 hours, is subsequently placed in alumina crucible and puts into Muffle furnace in drying baker at 60 DEG C, Calcine 30-60 minute at 300-400 DEG C.
CN201610069118.9A 2016-02-02 2016-02-02 Au nano particle/MoO3 nanorod heterojunction material with trimethylamine sensitizing effect Pending CN105753051A (en)

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Publication number Priority date Publication date Assignee Title
CN110308136A (en) * 2019-06-25 2019-10-08 中国计量大学 A kind of noble metal and MoO3The preparation method and application of self-assembled material
CN114314666A (en) * 2022-01-19 2022-04-12 中国科学院地球环境研究所 Oxygen vacancy type nano molybdenum trioxide antibacterial agent and preparation method thereof

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CN103449524A (en) * 2013-08-23 2013-12-18 东华大学 Molybdenum oxide based nano photothermal conversion material and preparation method thereof
CN105148910A (en) * 2015-07-17 2015-12-16 济南大学 Preparation method for hexagonal flaky molybdenum oxide loaded with gold nanometer particles

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CN101412541A (en) * 2007-10-19 2009-04-22 中国科学院大连化学物理研究所 Method for synthesizing rod-like and echinoid molybdena-based nano-material
CN103449524A (en) * 2013-08-23 2013-12-18 东华大学 Molybdenum oxide based nano photothermal conversion material and preparation method thereof
CN105148910A (en) * 2015-07-17 2015-12-16 济南大学 Preparation method for hexagonal flaky molybdenum oxide loaded with gold nanometer particles

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110308136A (en) * 2019-06-25 2019-10-08 中国计量大学 A kind of noble metal and MoO3The preparation method and application of self-assembled material
CN110308136B (en) * 2019-06-25 2021-07-30 中国计量大学 Preparation method and application of noble metal and MoO3 self-assembly material
CN114314666A (en) * 2022-01-19 2022-04-12 中国科学院地球环境研究所 Oxygen vacancy type nano molybdenum trioxide antibacterial agent and preparation method thereof

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Application publication date: 20160713