CN105152215A - Preparation method for Au nanometer particle modified flower-ball-shaped molybdenum disulfide with three-dimensional hierarchical structure - Google Patents
Preparation method for Au nanometer particle modified flower-ball-shaped molybdenum disulfide with three-dimensional hierarchical structure Download PDFInfo
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Abstract
The invention provides a preparation method for an Au-modified flower-ball-shaped molybdenum disulfide microsphere with a three-dimensional hierarchical structure, belonging to the technical field of preparation technology of inorganic advanced nanometer materials. The Au-modified flower-ball-shaped molybdenum disulfide with the three-dimensional hierarchical structure is synthesized by reaction at room temperature with chloroauric acid, sodium borohydride, L-lysine and prepared molybdenum disulfide as raw materials. A preparation method concretely comprises the following steps: dispersing the prepared molybdenum disulfide into a certain volume of deionized water, then 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 a muffle furnace, and carrying out calcining at a certain temperature for a certain time so as to obtain the Au-modified flower-ball-shaped molybdenum disulfide microsphere with the three-dimensional hierarchical structure. 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 flower-ball-shaped molybdenum disulfide microsphere with the three-dimensional hierarchical structure 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 three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
Background technology
Class Graphene molybdenumdisulphide (MoS
2) compound with " sandwich " laminate structure that is made up of the single or multiple lift molybdenumdisulphide of hexagonal system, the three layers of S-Mo-S covalent linkage separated by Van der Waals space are tightly packed to be formed, the Van der Waals space of its interlayer can allow that external reactant carries out insertion reaction, material of main part expands along C crystallographic direction, causes the volume change of material.Class Graphene MoS
2because of microtexture and reason, the voltinism matter of its uniqueness, still there is in the shortcoming overcoming zero band gap Graphene the lot of advantages of Graphene simultaneously, thus gather around in various fields such as secondary cell, field-effect transistor, sensor, electroluminescent, electricity storages and have broad application prospects.Different from the Graphene with two-dimensional layered structure, MoS
2more stable in the air atmosphere of certain temperature range, therefore, molybdenumdisulphide based composites will have more practical significance in fields such as photocatalysis technology, gas sensing techniques and devices.
Jin Yixiang is acknowledged as chemically inert, and it is very weak to the chemical adsorption capacity of oxygen and other gases.From thermodynamics, its oxide compound Au
2o
3unstable.Secondly, the electronegativity of gold is greater than every other metal, only than sulphur and iodine element slightly more just.And due to the Standard Electrode Potentials of Au+/Au0 be+1.691V, it is in fact also large than oxygen element to the affinity of electronics, and therefore it is difficult to oxidizing reaction occurs.Finally, due on periodictable/lanthanide contraction 0 effect, the atomic radius being positioned at the gold of the 3rd transition system is less than the silver atoms of the second transition system, and its fusing point and enthalpy of sublimation are all than the height of silver, and the interaction force between the atom of explanation own is stronger.These characteristics above-mentioned cause chemical reaction ability and the low major cause of catalytic activity of gold.But along with metallics particle diameter reduces, surface atom number increases, and the electronic property of itself will change, thus cause its chemistry and physical properties to occur sudden change, catalytic activity also increases to some extent.In recent years, researchers found that golden loaded catalyst can to photochemical catalysis, and there is excellent performance in the fields such as air-sensitive, (Xu Jiaqiang, Han Jianjun, Xie Bing, the Liu Yun .Au-In such as Xu Jiaqiang
2o
3the performance of CO gas sensor and study mechanism. sensing technology journal, 2007,20 (3)) synthesize In by chemical precipitation method
2o
3nano particle, better, average particle size particle size is at 20 ~ 40nm for its size uniform, dispersiveness.300 DEG C time, 2% gold medal doping has good sensitization to Indium sesquioxide base CO sensor, and to H
2there is no obvious sensitization.The catalysis detection etc. of gold has been studied into a compelling new direction in the world, and relevant new discovery continues to bring out, and Yang Jianjun etc. (Yang Jianjun, He Panke, Zhang Min, Wang Xiaohui, Yang Dongmei, Jin Zhensheng. the Au/TiO of Ozone Photocatalytic
2catalyzer [P]. Chinese patent: CN200510107365.5,2005-12-30) prepare Au/TiO
2matrix material, is suitable for the elimination of ozone in indoor air-purification device.Load type gold catalyst all demonstrates good catalytic activity to many important reactions such as Oxidation of Carbon Monoxide, hydrocarbon catalytic burning, epoxidation of propylene, liquid-phase selective oxidation, catalytic hydrogenation reactions, imply that Au catalyst has broad application prospects.
Research about class graphene-structured molybdenumdisulphide/gold nano grain matrix material is all at home and abroad ground zero, (the Wang Xinhuan such as Wang Xinhuan, Han Qiusen, Yang Rong, Wang Chen. a kind of molybdenumdisulphide/gold nanorods matrix material, Preparation method and use [P]. Chinese patent: CN201410815045.4,2014-12-23) prepared molybdenumdisulphide/gold nanorods matrix material, gold nanorods at about 30nm, and is pointed out for photo-thermal therapy.But other relevant research reports seldom.Therefore, gold grain load-type composite material and the application thereof of exploring smaller szie 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 molybdenumdisulphide/gold nano grain, present method production technique is simple, and productive rate is high, non-environmental-pollution, has good scientific research prospect and using value.Gained molybdenumdisulphide/gold nano grain regular appearance, can be used for the fields such as chemical industry catalysis, photochemical catalysis, gas sensor.
Technical scheme of the present invention is: be distributed in the deionized water of certain volume by a certain amount of molybdenum disulfide powder, add the chlorauric acid solution of certain mol proportion, 1B solution and sodium borohydride solution fully mix, normal-temperature reaction certain hour, centrifugation, washing, dry, under being placed in retort furnace certain temperature in air, thermal treatment can obtain Au modification three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
Concrete synthesis step is as follows:
(1) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(2) the molybdenum disulfide powder ultrasonic disperse prepared by 0.01-0.1g is in 10-50ml deionized water;
(3) in the solution in step (2), add 1-5ml chlorauric acid solution and 1-5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 10-30min that hydrochloro-auric acid and sodium borohydride solution obtain mol ratio; Dropwise add 0.1-1.0ml sodium borohydride solution, magnetic agitation 10-30min;
(4) reacted product whizzer is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in loft drier by step (4) gained solid product, 60 DEG C of dry 5-10 hour, are then placed in retort furnace, thermal treatment 30min-120min at 300 DEG C, obtain Au and modify three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
After the present invention adopts technique scheme, mainly contain following effect:
(1) the present invention's each step in preparation process does not produce hazardous and noxious substances, and be conducive to environment 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 scale operation;
(3) Au that prepared by the present invention modifies three-dimensional hierarchical structure flower ball-shaped mos2 microsphere regular appearance, and specific surface area is large and gold grain particle diameter is little, is uniformly dispersed, can be used for the field such as chemical industry catalysis, photocatalyst gas sensor.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of three-dimensional hierarchical structure flower ball-shaped mos2 microsphere in embodiment 1
Fig. 2 is the FESEM figure of three-dimensional hierarchical structure flower ball-shaped mos2 microsphere in embodiment 1
Fig. 3 is the X ray diffracting spectrum that in embodiment 1, Au modifies three-dimensional hierarchical structure flower ball-shaped mos2 microsphere
Fig. 4 is the FESEM figure that in embodiment 1, Au modifies three-dimensional hierarchical structure flower ball-shaped mos2 microsphere
Fig. 5 is the EDS energy spectrogram that in embodiment 1, Au modifies three-dimensional hierarchical structure flower ball-shaped mos2 microsphere
Fig. 6 is the FESEM figure that in embodiment 2, Au modifies three-dimensional hierarchical structure flower ball-shaped mos2 microsphere
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment
Embodiment 1
(1) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(2) the molybdenum disulfide powder ultrasonic disperse prepared by 0.05g is in 15ml deionized water;
(3) in the solution in step (2), add 1.5ml chlorauric acid solution and 1.5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 20min that hydrochloro-auric acid and sodium borohydride solution obtain mol ratio; Dropwise add 0.2ml sodium borohydride solution, magnetic agitation 20min;
(4) reacted product whizzer is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in loft drier by step (4) gained solid product, 60 DEG C of dryings 8 hours, are then placed in retort furnace, thermal treatment 30min at 300 DEG C, obtain Au and modify three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
The X-ray diffractogram collection of illustrative plates of three-dimensional hierarchical structure flower ball-shaped mos2 microsphere used in embodiment 1 as shown in Figure 1, the position of all diffraction peaks of the XRD figure spectrum of sample is consistent with international standard card PDF#65-0160, shows that sample used is exactly molybdenumdisulphide.Through the FESEM picture of field emission scanning electron microscope shooting gained, as shown in Figure 2, can find out that the pattern of molybdenumdisulphide is the flower ball-shaped of three-dimensional hierarchical structure, regular appearance.
The X-ray diffractogram collection of illustrative plates of molybdenumdisulphide/gold nano grain three-dimensional hierarchical structure microballoon that embodiment 1 is prepared as shown in Figure 3, the position of all diffraction peaks of the XRD figure of the sample prepared by the present invention spectrum is adopted to be consistent with the diffraction peak of molybdenumdisulphide and gold, without other assorted peaks, show that prepared sample is composite molybdenum disulfide/gold nano grain.Through the FESEM picture of field emission scanning electron microscope shooting gained, as shown in Figure 4, can find out molybdenumdisulphide/gold nano grain three-dimensional hierarchical structure regular appearance, gold grain is of a size of below 10nm and is uniformly dispersed.Through EDS energy-spectrum scanning gained result as shown in Figure 5, the existence of gold (Au), molybdenum (Mo), sulphur (S) three kinds of elements can be found out, and the strength of signal of gold is very high, comprehensive XRD, SEM, EDS result illustrates that gold grain successfully loads on molybdenum disulfide nano sheet.
Embodiment 2
(1) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(2) the molybdenum disulfide powder ultrasonic disperse prepared by 0.01g is in 10ml deionized water;
(3) in the solution in step (2), add 1ml chlorauric acid solution and 1mlL-lysine solution, wherein, it is 1:1, magnetic agitation 10min that hydrochloro-auric acid and sodium borohydride solution obtain mol ratio; Dropwise add 0.1ml sodium borohydride solution, magnetic agitation 10min;
(4) reacted product whizzer is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in loft drier by step (4) gained solid product, 60 DEG C of dryings 5 hours, are then placed in retort furnace, thermal treatment 30min at 300 DEG C, obtain Au and modify three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
Molybdenumdisulphide/gold nano grain prepared by embodiment 2 as shown in Figure 6, can find out that obtained molybdenumdisulphide/gold nano grain three-dimensional hierarchical structure compound is good.
Embodiment 3
(1) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(2) the molybdenum disulfide powder ultrasonic disperse prepared by 0.03g is in 20ml deionized water;
(3) in the solution in step (2), add 2ml chlorauric acid solution and 2mlL-lysine solution, wherein, it is 1:1, magnetic agitation 20min that hydrochloro-auric acid and sodium borohydride solution obtain mol ratio; Dropwise add 0.2ml sodium borohydride solution, magnetic agitation 20min;
(4) reacted product whizzer is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in loft drier by step (4) gained solid product, 60 DEG C of dryings 6 hours, are then placed in retort furnace, thermal treatment 60min at 300 DEG C, obtain Au and modify three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
Embodiment 4
(1) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(2) the molybdenum disulfide powder ultrasonic disperse prepared by 0.08g is in 30ml deionized water;
(3) in the solution in step (2), add 3ml chlorauric acid solution and 3mlL-lysine solution, wherein, it is 1:1, magnetic agitation 30min that hydrochloro-auric acid and sodium borohydride solution obtain mol ratio; Dropwise add 5.0ml sodium borohydride solution, magnetic agitation 30min;
(4) reacted product whizzer is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in loft drier by step (4) gained solid product, 60 DEG C of dryings 8 hours, are then placed in retort furnace, thermal treatment 30min at 300 DEG C, obtain Au and modify three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
Embodiment 5
(1) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(2) the molybdenum disulfide powder ultrasonic disperse prepared by 0.1g is in 50ml deionized water;
(3) in the solution in step (2), add 5ml chlorauric acid solution and 5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 30min that hydrochloro-auric acid and sodium borohydride solution obtain mol ratio; Dropwise add 1.0ml sodium borohydride solution, magnetic agitation 30min;
(4) reacted product whizzer is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in loft drier by step (4) gained solid product, 60 DEG C of dryings 10 hours, are then placed in retort furnace, thermal treatment 120min at 300 DEG C, obtain Au and modify three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
Claims (1)
1. Au modifies a preparation method for three-dimensional hierarchical structure flower ball-shaped mos2 microsphere, and concrete synthesis step is as follows:
(1) 0.01M chlorauric acid solution is prepared, the 1B solution of 0.01M and 0.1M sodium borohydride solution;
(2) the molybdenum disulfide powder ultrasonic disperse prepared by 0.01-0.1g is in 10-50ml deionized water;
(3) in the solution in step (2), add 1-5ml chlorauric acid solution and 1-5mlL-lysine solution, wherein, it is 1:1, magnetic agitation 10-30min that hydrochloro-auric acid and sodium borohydride solution obtain mol ratio; Dropwise add 0.1-1.0ml sodium borohydride solution, magnetic agitation 10-30min;
(4) reacted product whizzer is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(5) be positioned in loft drier by step (4) gained solid product, 60 DEG C of dry 5-10 hour, are then placed in retort furnace, thermal treatment 30min-120min at 300 DEG C, obtain Au and modify three-dimensional hierarchical structure flower ball-shaped mos2 microsphere.
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