CN105148910A - Preparation method for hexagonal flaky molybdenum oxide loaded with gold nanometer particles - Google Patents
Preparation method for hexagonal flaky molybdenum oxide loaded with gold nanometer particles Download PDFInfo
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- CN105148910A CN105148910A CN201510418713.4A CN201510418713A CN105148910A CN 105148910 A CN105148910 A CN 105148910A CN 201510418713 A CN201510418713 A CN 201510418713A CN 105148910 A CN105148910 A CN 105148910A
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Abstract
The invention provides a preparation method for Au-modified hexagonal flaky molybdenum oxide, belonging to the technical field of preparation technology of inorganic advanced nanometer materials. The An-modified hexagonal flaky molybdenum oxide material is synthesized by reaction at room temperature with chloroauric acid, sodium borohydride, L-lysine and prepared hexagonal flaky molybdenum oxide as raw materials. A preparation method concretely comprises the following steps: placing a precursor, i.e., molybdenum disulfide, into a muffle furnace and carrying out calcining at a certain temperature under an oxygen atmosphere for a certain time so as to obtain the hexagonal flaky molybdenum oxide, then dispersing the hexagonal flaky molybdenum oxide into a certain volume of deionized water, adding the chloroauric acid and L-lysine in a certain molar ratio, carrying out full mixing, then adding a certain amount of a sodium borohydride solution, and carrying out full mixing under stirring; and after a certain time of reaction at room temperature, carrying out centrifugal separation, washing and drying, then placing an obtained dried sample in the muffle furnace, and carrying out calcining at a certain temperature for a certain time so as to obtain the Au-modified hexagonal flaky molybdenum oxide. The method provided by the invention has the advantages of low cost, simple production process, high yield, no environmental pollution, and facilitation to large-scale industrial production. The obtained Au-modified hexagonal flaky molybdenum oxide has regular morphology and can be applied in the fields of chemical catalysis, photocatalyst gas sensors, etc.
Description
Technical field
The invention belongs to inorganic advanced technical field of nano-composite material preparation technology, particularly relate to the preparation method that Au modifies hexagonal flake molybdenum oxide.
Background technology
Molybdenum oxide is a kind of N-type semiconductor of broad-band gap, exists mutually: orthorhombic phase (α MoO with 3 kinds of common things
3), six side's phase (h-MoO
3) and monoclinic phase, the former is thermodynamically stable phase, is thermodynamically metastable phases both rear.Compared with thermodynamics stable state, metasable state usually shows more excellent physical and chemical activity, metasable state six side phase molybdenum trioxide (h-MoO
3) there is photic and electro optical phenomenon, can be used as the excellent photoelectron material of some Military Application technology.At present, nanometer MoO is prepared
3method have solid phase method, hydro-thermal method, the precipitation method, chemical vapour deposition technique etc., comparatively speaking, use hydro-thermal rule can obtain the nanometer MoO of uniform-dimension
3, product good dispersion, cost is low, and technique is simple and have good repeatability, thus obtains using comparatively widely.
Noble-metal-supported is one of conventional modified method, noble metal forms active centre at semiconductor surface, and its sky d track can accept electronics, is conducive to improving absorption, redox ability, promote separation of charge, thus improve the performance such as photocatalysis, air-sensitive of material.Jin Yixiang is acknowledged as chemically inert, from thermodynamics, and its oxide Au
2o
3unstable.In recent years, researchers are studying fields such as golden loaded catalyst, gas sensors always, Wang Xinhuan etc. (Wang Xin ring Han Qiu gloomy Yang Rong Wang Chen. a kind of molybdenum bisuphide/gold nanorods composite, Preparation method and use [P]. Chinese patent: CN201410815045.4,2014-12-13) prepare molybdenum bisuphide/gold nanorods composite, for photo-thermal therapy.(He Panke, Yang Jianjun, Yang Dongmei, Wang Xiaohui, a quick .Au/TiO such as He Panke
2photocatalysis Decomposition ozone, catalysis journal, 2006,27 (1)) adopt deposition-precipitation to prepare Au/TiO
2catalyst, more effectively facilitates O
3decomposition.(ZhenZhu, JialunChang, RenjangWu, the Fastozonedetectionbyusingacore-shellAuTiO such as ZhenZhu
2sensoratroomtemperature.SensorsandActuatorsB:Chemical, 214 (2015) 56-62) prepare AuTiO
2gas sensor, and at room temperature measure O
3response and recovery time be 3s and 20s, in air-sensitive, had good application.The catalysis detection etc. of gold has been studied into a compelling new direction in the world, relevant new discovery continues to bring out, (the Qin Yao such as Qin Yao, Yang Jinhu, Jin Chao, Li Ying, Li Jie, Shi Donglu. the preparation method [P] of dandelion shape nucleocapsid structure AuZnO heterojunction photocatalyst. Chinese patent: CN201310400997.5,2013-09-05) prepare Au nano particle ZnO senior nucleocapsid AuZnO hetero-junctions catalyst outside inside, have good application prospect in fields such as photocatalytic degradation environmental contaminants and solar hydrogen makings.
Research about gold nano grain/molybdenum oxide composite is all at home and abroad ground zero, and relevant research report seldom.Therefore, exploration gold nano grain/molybdenum oxide composite and application thereof are directions being worth making great efforts research.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of molybdenum oxide/gold nano grain, this method production technology is simple, and productive rate is high, non-environmental-pollution, has good scientific research prospect and using value.Gained molybdenum oxide/gold nano grain regular appearance, can be used for the fields such as chemical industry catalysis, photocatalysis, gas sensor.
Technical scheme of the present invention is: presoma molybdenum bisuphide is put into Muffle furnace and under the oxygen atmosphere of uniform temperature, calcine certain hour obtain hexagonal flake molybdenum oxide, then molybdenum oxide is distributed in the deionized water of certain volume, add the chlorauric acid solution of certain mol proportion, 1B solution and sodium borohydride solution fully mix, normal-temperature reaction certain hour, centrifugation, washing, drying, is placed in the preparation method that heat treatment under Muffle furnace uniform temperature can obtain a kind of hexagonal flake molybdenum oxide load gold nano grain in air.
Concrete synthesis step is as follows:
(1) 1g presoma molybdenum bisuphide is put into Muffle furnace to calcine under oxygen atmosphere, calcining heat is 360 DEG C-450 DEG C, and calcination time is 120min-200min;
(2) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(3) the molybdenum oxide powder ultrasonic disperse prepared by 0.01g-0.1g is in 10ml-30ml deionized water;
(4) in the solution in step (3), add 1ml-5ml chlorauric acid solution and 1ml-5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 20-40min that gold chloride and sodium borohydride solution obtain mol ratio; Dropwise add 0.1ml-2.0ml sodium borohydride solution, magnetic agitation 10min-30min; Reacted product centrifuge is carried out Separation of Solid and Liquid, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in drying box by step (4) gained solid product, 60 DEG C of dry 6h-12h, are then placed in Muffle furnace, heat treatment 30min-60min at 300 DEG C, obtain Au and modify hexagonal flake molybdenum oxide.
After the present invention adopts technique scheme, mainly contain following effect:
(1) the present invention's each step in preparation process does not produce poisonous and harmful substance, and be conducive to environmental protection, and the hydro-thermal reaction time is short, efficiency is high;
(2) the inventive method is simple, and easy to operate, the plant-scale equipment is simple and easy, is easy to industrialization large-scale production;
(3) Au that prepared by the present invention modifies hexagonal flake molybdenum oxide microballoon regular appearance, and gold grain particle diameter is little, is uniformly dispersed, and can be used for the field such as chemical industry catalysis, photochemical catalyst gas sensor.
Accompanying drawing explanation
Fig. 1 is the SEM figure of hexagonal flake molybdenum oxide in embodiment 1
Fig. 2 is the X ray diffracting spectrum that in embodiment 1, Au modifies hexagonal flake molybdenum oxide
Fig. 3 is the FESEM figure that in embodiment 1, Au modifies hexagonal flake molybdenum oxide
Fig. 4 is the EDS energy spectrogram that in embodiment 1, Au modifies hexagonal flake molybdenum oxide
Fig. 5 is the FESEM figure that in embodiment 2, Au modifies hexagonal flake molybdenum oxide
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Detailed description of the invention
Embodiment 1
(1) 1g presoma molybdenum bisuphide is put into Muffle furnace to calcine under oxygen atmosphere, calcining heat is 400 DEG C, and calcination time is 180min;
(2) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(3) the molybdenum oxide powder ultrasonic disperse prepared by 0.05g is in 15ml deionized water;
(4) in the solution in step (3), add 1.5ml chlorauric acid solution and 1.5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 30min that gold chloride and sodium borohydride solution obtain mol ratio; Dropwise add 0.2ml sodium borohydride solution, magnetic agitation 20min; Reacted product centrifuge is carried out Separation of Solid and Liquid, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in drying box by step (4) gained solid product, 60 DEG C of dry 8h, are then placed in Muffle furnace, heat treatment 30min at 300 DEG C, obtain Au and modify hexagonal flake molybdenum oxide.
Hexagonal flake molybdenum oxide used in embodiment 1, through the FESEM picture of field emission scanning electron microscope shooting gained, as shown in Figure 1, can find out that the pattern of molybdenum oxide is hexagonal flake.The X-ray diffractogram collection of illustrative plates of hexagonal flake molybdenum oxide/gold nano grain that embodiment 1 is prepared as shown in Figure 2, the position of all diffraction maximums of the XRD collection of illustrative plates of the sample prepared by the present invention is adopted to be consistent with the diffraction maximum of molybdenum oxide (PDF#35-0609) and gold, without other assorted peaks, show that prepared sample is molybdenum oxide/gold nano grain composite.Through the FESEM picture of field emission scanning electron microscope shooting gained, as shown in Figure 3, can find out molybdenum oxide/gold nano grain regular appearance, gold grain is of a size of tens nanometers and is uniformly dispersed.Through EDS energy-spectrum scanning gained result as shown in Figure 4, can find out the existence of gold (Au), molybdenum (Mo), oxygen (O) three kinds of elements, and the signal strength signal intensity of gold is very high, comprehensive XRD, SEM, EDS result illustrates that gold grain successfully loads in molybdenum oxide six square piece.
Embodiment 2
(1) 1g presoma molybdenum bisuphide is put into Muffle furnace to calcine under oxygen atmosphere, calcining heat is 380 DEG C, and calcination time is 150min;
(2) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(3) the molybdenum oxide powder ultrasonic disperse prepared by 0.1g is in 30ml deionized water;
(4) in the solution in step (3), add 3ml chlorauric acid solution and 3mlL-lysine solution, wherein, it is 1:1, magnetic agitation 30min that gold chloride and sodium borohydride solution obtain mol ratio; Dropwise add 0.5ml sodium borohydride solution, magnetic agitation 30min; Reacted product centrifuge is carried out Separation of Solid and Liquid, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in drying box by step (4) gained solid product, 60 DEG C of dry 6h, are then placed in Muffle furnace, heat treatment 30min at 300 DEG C, obtain Au and modify hexagonal flake molybdenum oxide.
Molybdenum oxide/gold nano grain prepared by embodiment 2 as shown in Figure 5, can find out that obtained molybdenum oxide/gold nano grain compound is good.
Embodiment 3
(1) 1g presoma molybdenum bisuphide is put into Muffle furnace to calcine under oxygen atmosphere, calcining heat is 360 DEG C, and calcination time is 200min;
(2) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(3) the molybdenum oxide powder ultrasonic disperse prepared by 0.02g is in 10ml deionized water;
(4) in the solution in step (3), add 1ml chlorauric acid solution and 1mlL-lysine solution, wherein, it is 1:1, magnetic agitation 20min that gold chloride and sodium borohydride solution obtain mol ratio; Dropwise add 0.1ml sodium borohydride solution, magnetic agitation 10min; Reacted product centrifuge is carried out Separation of Solid and Liquid, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in drying box by step (4) gained solid product, 60 DEG C of dry 6h, are then placed in Muffle furnace, heat treatment 30min at 300 DEG C, obtain Au and modify hexagonal flake molybdenum oxide.
Embodiment 4
(1) 1g presoma molybdenum bisuphide is put into Muffle furnace to calcine under oxygen atmosphere, calcining heat is 390 DEG C, and calcination time is 150min;
(2) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(3) the molybdenum oxide powder ultrasonic disperse prepared by 0.08g is in 20ml deionized water;
(4) in the solution in step (3), add 2ml chlorauric acid solution and 2mlL-lysine solution, wherein, it is 1:1, magnetic agitation 40min that gold chloride and sodium borohydride solution obtain mol ratio; Dropwise add 0.3ml sodium borohydride solution, magnetic agitation 30min; Reacted product centrifuge is carried out Separation of Solid and Liquid, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in drying box by step (4) gained solid product, 60 DEG C of dry 12h, are then placed in Muffle furnace, heat treatment 40min at 300 DEG C, obtain Au and modify hexagonal flake molybdenum oxide.
Embodiment 5
(1) 1g presoma molybdenum bisuphide is put into Muffle furnace to calcine under oxygen atmosphere, calcining heat is 370 DEG C, and calcination time is 180min;
(2) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(3) the molybdenum oxide powder ultrasonic disperse prepared by 0.06g is in 15ml deionized water;
(4) in the solution in step (3), add 1.5ml chlorauric acid solution and 1.5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 20min that gold chloride and sodium borohydride solution obtain mol ratio; Dropwise add 0.1m sodium borohydride solution, magnetic agitation 10min; Reacted product centrifuge is carried out Separation of Solid and Liquid, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in drying box by step (4) gained solid product, 60 DEG C of dry 12h, are then placed in Muffle furnace, heat treatment 30min at 300 DEG C, obtain Au and modify hexagonal flake molybdenum oxide.
Claims (1)
1. a preparation method for the nano-particle modified hexagonal flake molybdenum oxide of Au, concrete synthesis step is as follows:
(1) 1g presoma molybdenum bisuphide is put into Muffle furnace to calcine under oxygen atmosphere, calcining heat is 360 DEG C-450 DEG C, and calcination time is 120min-200min;
(2) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(3) the molybdenum oxide powder ultrasonic disperse prepared by 0.01g-0.1g is in 10ml-30ml deionized water;
(4) in the solution in step (3), add 1ml-5ml chlorauric acid solution and 1ml-5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 20-40min that gold chloride and sodium borohydride solution obtain mol ratio; Dropwise add 0.1ml-2.0ml sodium borohydride solution, magnetic agitation 10min-30min; Reacted product centrifuge is carried out Separation of Solid and Liquid, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in drying box by step (4) gained solid product, 60 DEG C of dry 6h-12h, are then placed in Muffle furnace, heat treatment 30min-60min at 300 DEG C, obtain Au and modify hexagonal flake molybdenum oxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105753051A (en) * | 2016-02-02 | 2016-07-13 | 济南大学 | Au nano particle/MoO3 nanorod heterojunction material with trimethylamine sensitizing effect |
| CN110181072A (en) * | 2019-06-05 | 2019-08-30 | 南京邮电大学 | Morphology controllable hexagon gold/molybdenum disulfide nano-composite material preparation method |
| CN112076716A (en) * | 2020-09-04 | 2020-12-15 | 江西善纳新材料科技有限公司 | Composite phase nano molybdenum trioxide adsorbent and preparation method thereof |
| CN113617353A (en) * | 2021-08-02 | 2021-11-09 | 常州大学 | Preparation method of silicon carbide-based silver nano catalyst and application of silicon carbide-based silver nano catalyst in synthesis of ethylene oxide |
| CN113697857A (en) * | 2021-09-14 | 2021-11-26 | 河北地质大学 | Preparation method and application of two-dimensional flaky molybdenum oxide nano material |
| CN114609197A (en) * | 2022-03-25 | 2022-06-10 | 电子科技大学 | Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor |
| CN114931948A (en) * | 2022-03-25 | 2022-08-23 | 山东大学 | Potassium intercalation molybdenum oxide nano array material and preparation method and application thereof |
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Cited By (11)
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| CN105753051A (en) * | 2016-02-02 | 2016-07-13 | 济南大学 | Au nano particle/MoO3 nanorod heterojunction material with trimethylamine sensitizing effect |
| CN110181072A (en) * | 2019-06-05 | 2019-08-30 | 南京邮电大学 | Morphology controllable hexagon gold/molybdenum disulfide nano-composite material preparation method |
| CN112076716A (en) * | 2020-09-04 | 2020-12-15 | 江西善纳新材料科技有限公司 | Composite phase nano molybdenum trioxide adsorbent and preparation method thereof |
| CN113617353A (en) * | 2021-08-02 | 2021-11-09 | 常州大学 | Preparation method of silicon carbide-based silver nano catalyst and application of silicon carbide-based silver nano catalyst in synthesis of ethylene oxide |
| CN113617353B (en) * | 2021-08-02 | 2023-09-22 | 常州大学 | Preparation method of silicon carbide-based silver nano catalyst and application of silicon carbide-based silver nano catalyst in ethylene oxide synthesis |
| CN113697857A (en) * | 2021-09-14 | 2021-11-26 | 河北地质大学 | Preparation method and application of two-dimensional flaky molybdenum oxide nano material |
| CN113697857B (en) * | 2021-09-14 | 2023-01-24 | 河北地质大学 | Preparation method and application of two-dimensional flaky molybdenum oxide nano material |
| CN114609197A (en) * | 2022-03-25 | 2022-06-10 | 电子科技大学 | Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor |
| CN114931948A (en) * | 2022-03-25 | 2022-08-23 | 山东大学 | Potassium intercalation molybdenum oxide nano array material and preparation method and application thereof |
| CN114931948B (en) * | 2022-03-25 | 2023-04-07 | 山东大学 | Potassium intercalation molybdenum oxide nano array material and preparation method and application thereof |
| CN114609197B (en) * | 2022-03-25 | 2023-11-21 | 电子科技大学 | Gas-sensitive material, preparation method and NH (NH) thereof 3 Application in gas sensor |
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