CN104150536A - Preparation method and application of MoO2 powder with favorable photoelectric properties - Google Patents

Preparation method and application of MoO2 powder with favorable photoelectric properties Download PDF

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CN104150536A
CN104150536A CN201410385575.XA CN201410385575A CN104150536A CN 104150536 A CN104150536 A CN 104150536A CN 201410385575 A CN201410385575 A CN 201410385575A CN 104150536 A CN104150536 A CN 104150536A
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moo
powder
preparation
solution
photoelectric properties
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CN104150536B (en
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李靖
朱杨杨
陈艳
堵锡华
蔡可迎
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Xuzhou University of Technology
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Xuzhou University of Technology
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Abstract

The invention provides a preparation method and application of MoO2 with favorable photoelectric properties. The preparation method comprises the following steps: S10: an ammonium molybdate aqueous solution with concentration of 25 mg/L is prepared; S20: acetate and glucose are added into the ammonium molybdate solution and stirred to obtain a uniformly mixed solution; S30: the solution obtained in the S20 is sealed in a reaction kettle for heating and subjected to reduction reaction to obtain sediments; S40: the sediments obtained in the S30 are subjected to suction filtration and washing through the adoption of a reagent to obtain brownish-black sediments; S50: the brownish-black sediments obtained in the S40 is dried and grinded to obtain MoO2 powder. According to the preparation method provided by the invention, the prepared MoO2 powder has favorable absorbability and photo-catalytic activity on hexavalent chromium in water and the MoO2 further has a favorable circular volt-ampere property.

Description

The MoO with good photoelectric properties 2the preparation method of powder and application
[technical field]
The present invention relates to a kind of MoO 2the preparation method of powder, is specifically related to a kind of MoO with good photoelectric properties 2the preparation method of powder and application.
[background technology]
MoO 2it is a kind of broad-band gap transition metal oxide with high-melting-point, high chemical stability, high conductivity.At MoO 2the octahedral structure of middle existence distortion has determined that lithium ion is at MoO 2in the speed that is embedded in and deviates from, MoO simultaneously 2there is the reversible advantage of capacity, make MoO 2become the study hotspot of electrochemical field, can be used as field emmision material, sensor, photochromic chromogenic device, electric chemical super capacitor etc.But relevant MoO 2report as sorbing material and semiconductor light-catalyst processing water pollutant is comparatively rare.
Because the performance of material depends on the character such as granular size, crystal formation, crystallinity, specific surface area of material, and these character depend on synthetic method.Nowadays MoO 2preparation method more; some synthetic method needs vacuum reaction and protection of inert gas; the presoma that need to utilize having reacts; this not only needs harsh reaction conditions; also need accurate reaction kit; preparation method is complicated, and restive and adjustment reaction conditions, and the MoO preparing 2performance is not fine.
[summary of the invention]
For the problems referred to above, the invention provides a kind of MoO with good photoelectric properties 2the preparation method of powder and application, MoO of the present invention 2that powder preparation method has is simple to operate, be convenient to control and adjust reaction conditions, the MoO making by the method for the invention 2powder has good cyclic voltammetric performance, photocatalysis performance and absorption property, can be used as preparing sorbing material and semiconductor light-catalyst.
A kind of MoO with good photoelectric properties 2the preparation method of powder, comprises the following steps:
S10: the ammonium molybdate aqueous solution that compound concentration is 25mg/L;
S20: add acetic acid and glucose in ammonium molybdate solution, and stir, obtain the solution mixing;
S30: step S20 gained reaction soln is sealed in reactor and is heated, obtain throw out;
S40: adopt reagent to carry out filtering and washing processing step S30 gained throw out, obtain brownish black precipitation;
S50: step S40 gained brownish black precipitation is carried out to drying treatment, grind and obtain MoO 2powder;
Described MoO 2powder is prepared from according to 1g ammonium molybdate proportioning 34ml deionized water, 4ml acetic acid, 1g glucose.
Especially, the reduction reaction that described step S30 occurs is carried out in the stainless steel cauldron of poly-four vinyl liner.
Especially, in described step S40, suction filtration is processed and is comprised:
A: adopt deionized water lotion 4-6 time;
B: adopt dehydrated alcohol lotion 1-2 time.
A kind of MoO with good photoelectric properties making according to aforesaid method 2the application of powder in preparing sorbing material and semiconductor light-catalyst.
Compared to prior art, MoO provided by the invention 2powder is prepared by hydrothermal synthesis method, and that this preparation method has advantages of is simple to operate, be convenient to control and adjust reaction conditions, by the synthetic MoO of this method 2powder has the following advantages:
1, MoO 2powder particle size homogeneous;
2, MoO 2cyclic voltammetric functional, can be used for the exploitation of lithium ion battery;
3, good to chromic absorption property and photocatalysis performance in water, can be used for semiconductor light-catalyst and process water pollutant.
[accompanying drawing explanation]
Fig. 1 is the embodiment of the present invention and comparative example MoO 2powder X-ray powder diagram;
Fig. 2 is the embodiment of the present invention and comparative example MoO 2powder field emission scanning electron microscope figure;
Fig. 3 is the embodiment of the present invention and comparative example MoO 2powder infrared absorption spectrum figure;
Fig. 4 is the embodiment of the present invention and comparative example MoO 2powder fluorescence spectrum figure;
Fig. 5 is the embodiment of the present invention and comparative example MoO 2adsorption property comparison diagram under powder closed black dark situation;
Fig. 6 is MoO of the present invention 2powder character comparison diagram of Cr (VI) in different amounts planar water under airtight dark;
Fig. 7 is the embodiment of the present invention and comparative example MoO 2powder tungsten lamp irradiates lower photocatalytic activity comparison diagram;
Fig. 8 is MoO of the present invention 2the catalytic activity comparison diagram of powder photo catalytic reduction Cr (VI) under luminescent lamp (Fluorescentlamp) and xenon lamp (Xe lamp) irradiation;
Fig. 9 is MoO of the present invention 2the cyclic voltammogram that powder embodiment obtains through 100 circulations.
[embodiment]
Comparative example:
A: ammonium molybdate 1g, deionized water 34ml, hydrochloric acid 4ml, ethylene glycol 2ml.
Preparation method:
S10: the ammonium molybdate aqueous solution that compound concentration is 25mg/L;
First take 1g ammonium molybdate and put into the stainless steel cauldron of poly-four vinyl liner; Measure afterwards 34ml deionized water and add in above-mentioned stainless steel cauldron, obtain the mixing solutions of ammonium molybdate and deionized water; Then the mixing solutions of ammonium molybdate and deionized water is carried out to magnetic agitation it is mixed, the ammonium molybdate aqueous solution that acquisition concentration is 25mg/L, churning time is 3min;
S20: measure respectively 4ml hydrochloric acid, 2ml ethylene glycol, add in above-mentioned stainless steel cauldron, proceed magnetic agitation, obtain the solution mixing, churning time is 3min;
S30: step S20 gained solution is sealed in described stainless steel cauldron, be positioned over afterwards in electric oven and heat 12h at 190 ℃ of temperature, make solution carry out sufficient reduction reaction, question response system naturally cools to room temperature, obtain brownish black throw out, adopt the stainless steel cauldron of poly-four vinyl liner to play a protective role in heat-processed to solution, it should be noted that: in actual fabrication process, Heating temperature and heat-up time can suitably be adjusted according to practical situation herein;
S40: the filtering and washing of step S30 gained throw out being carried out to deionized water wash 4-6 time, absolute ethanol washing 1-2 time is processed, the brownish black that obtains washes clean precipitates; Adopt deionized water wash to remove other foreign ions residual in described black precipitate afterwards 4-6 time, adopting the object of absolute ethanol washing is to obtain dry MoO after guaranteeing to heat 5h at 100 ℃ 2powder;
S50: step S40 gained brownish black precipitation is put in electric oven and is dried 5h under the condition of 100 ℃, grind and obtain MoO 2powder it should be noted that herein: in actual fabrication process, drying temperature and time of drying can suitably be adjusted according to practical situation.
B: ammonium molybdate 1g, deionized water 34ml, hydrochloric acid 4ml, glucose 1g.
Preparation method is identical with comparative example a, repeats no more herein.
Embodiment:
C: ammonium molybdate 1g, deionized water 34ml, acetic acid 4ml, glucose 1g.
Preparation method is identical with comparative example a, repeats no more herein.
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment and experiment, to MoO provided by the invention 2the photoelectric properties of powder are verified.
1, select German Bruker AXS D8ADVANCEX-ray powder diffraction instrument (XRD, Cu K α radiation, 40kV, 200mA) to MoO 2powder carries out thing to be measured mutually, and measurement result as shown in Figure 1, is calculated MoO according to formula (1) 2particle diameter,
D＝Kλ/(βcosθ) (1)
In formula, D is that crystal grain is perpendicular to the particle diameter (nm) of crystal plane direction, K is constant (0.89), and λ is X-beam wavelength (0.15406nm), and β is for surveying sample diffraction peak halfwidth degree (must carry out two-wire proofreaies and correct and instrument factor correction) (rad), θ is diffraction angle (rad), according to the peak width at half height of (101) diffraction peak in Fig. 1, the particle diameter that calculates a is 0nm, and the particle diameter of b is 8nm, the particle diameter of embodiment c is 5nm, and the particle diameter of hence one can see that c is minimum.
2, adopt the Japanese Hitachi S-4800 of company type field emission scanning electron microscope (FESEM, 15kV) to MoO 2powder carries out morphology observation, obtains according to the observation field emission scanning electron microscope figure and sees Fig. 2, by Fig. 2, can observe made MoO 2product forms by nano particle, the MoO under different preparation conditions 2the size of nano particle is different, can measure the particle size of a in 18nm left and right by map scale, and the particle of b is in 10nm left and right, and the particle size of c is in 6nm left and right, and the particle size of hence one can see that c is minimum.
3, the optical and electrical properties of product:
3.1, Infrared Characterization:
As Fig. 3, can find out 623cm -1, 1620cm -1, 3455cm -1there is absorption peak, wherein 1620cm in place -1and 3455cm -1stretch and flexural vibration peak in the water molecules or the surface that are respectively surface adsorption.
3.2, Fluorescent Characterization:
There is very strong absorption peak in a as shown in Figure 4 at 360nm place, at 320nm and 715nm place, occur an extremely weak absorption peak; At 250nm and 493nm place, respectively there is a strong absorption peak in b; C only has absorption peak at 233nm place.By Fig. 4, can also be observed in a, b, c, the fluorescence intensity of c is minimum, this means MoO 2the light induced electron that powder produces under the irradiation of light source and the Compound Degree of photohole reduce, and in photocatalytic process, the utilization ratio of light induced electron or photohole improves.From photochemical catalysis experimental data, also proved that c has highlight catalytic active.
3.3, based on above to MoO 2adsorption property and the photocatalysis property thereof of powder are measured:
Determination experiment step:
1) sample that takes 0.3g, in the beaker of 500ml, adds 300mL50mg/L K 2cr 2o 7the aqueous solution or 300mL20mg/L MO (tropeolin-D) solution;
2) add stirrer, be placed on magnetic stirring apparatus, make it completely in the environment in airtight dark;
3) stir, every 10 or 20min for needle tubing extract suspension liquid 5ml out, be placed on centrifugal 30min in whizzer;
4) with dropper, carefully take out supernatant liquid standing in test tube;
5) being ready in advance 10ml volumetric flask, is the sulfuric acid that 0.5% phenylbenzene phosphinylidyne two hydrazine reagents and 9mL concentration are 0.2mol/L and 0.2mL concentration is housed in volumetric flask;
6) with 1ml transfer pipet, take out step 4) supernatant liquid add volumetric flask, mixed, the maximum absorption wavelength (λ max=540nm) of the violet complex forming at phenylbenzene phosphinylidyne two hydrazines and Cr (VI) after standing 5min locates to measure Cr (VI) absorbancy.
MoO 2photocatalytic activity to investigate be to get to after adsorption-desorption balance in dark absorption, reactor is placed under the irradiation of Different Light, according to the method for same measurement Cr (VI) concentration, carry out light-catalyzed reaction experiment.
The remaining rate of calculating Cr (VI) according to the absorbancy recording, calculation formula is formula (2):
Remaining rate=A of Cr (VI) t/ A 0(2)
In formula: A 0the absorbancy of etching solution during for dark absorption 0min, A tthe absorbancy of etching solution during for dark absorption tmin.Fig. 5 has provided a, b, the c absorption 300mL50mg/L K of 0.3g 2cr 2o 7the efficiency spectrogram of the aqueous solution or 300mL20mg/L MO (tropeolin-D) solution.A and b are all very weak to the adsorptive power of Cr (VI) as can be seen from Figure 5, also not high to the adsorptive power of MO, and c shows good absorption property in the process of absorption Cr (VI).
The c (0.3g-0.05g) that Fig. 6 has provided different amounts investigates the adsorption experiment of Cr in water (VI).As shown in Figure 6: when c consumption is 0.3g, 0.2g, when dark absorption 160min, in solution, the residual volume of Cr (VI) is 0, this means that the c of more consumption can adsorb certain density Cr (VI) completely; Relative c consumption is in the adsorption process of 0.05g and 0.1g, has reached adsorption equilibrium after certain hour, and the residual volume of Cr in solution (VI) maintains certain numerical value.
According to the adsorption experiment data of Fig. 6, determine time of equilibrium adsorption, the condition of airtight dark is adjusted into Different Light (tungsten lamp, luminescent lamp, xenon lamp) and irradiates, to investigate MoO 2photocatalysis performance.
Measure MoO 2photocatalysis property be to carry out under the precondition of dark absorption, when dark absorption reaches after adsorption equilibrium, suspension is placed in to the environment that tungsten lamp irradiates, press its absorbancy of step measurements of adsorption property, different from the time point that adsorption property is measured, after dark adsorption equilibrium, (being the initial time that tungsten lamp irradiates) is denoted as the time point of 0 minute, measure respectively 0min, 10min after turning on light, 20min, in light application time afterwards, at interval of 20min, get the absorbancy test of a little carrying out residual contamination substrate concentration in solution, afterwards according to the absorbancy recording, the concentration of calculating residual contaminants in solution according to formula (2) obtains Fig. 7.Under tungsten lamp irradiates, reducing as shown in Figure 7 a and b slightly raises to Cr (VI) reduction ratio, illustrates and all has certain photocatalytic activity; C is after tungsten lamp irradiates 260min, and in solution, the residual volume of tropeolin-D is 0, and apparently higher than the efficiency in dark adsorption process, this shows under the irradiation of tungsten lamp effectively MO in degradation water of c.
In order further to investigate Different Light, irradiate the photocatalysis property of lower c, above-mentioned tungsten lamp is irradiated and changes fluorescent lamp into, in order to contrast, comparative group is set simultaneously, comparative group adopts xenon lamp (to use spectral filter, elimination UV-light) irradiate, all the other conditions are identical with tungsten lamp illuminate condition, obtain Fig. 8, by Fig. 8, can find out clearly that c can reduce Cr (VI) under the irradiation of luminescent lamp within the relatively short time, and under the irradiation of xenon lamp, be without any effect, also just proved MoO 2under visible ray, do not there is photocatalytic activity.
4, MoO 2cyclic voltammetry test:
Experimental procedure:
1) polishing of solid electrode:
First deionized water, dehydrated alcohol for Graphite Electrodes are cleaned, use afterwards the aluminum oxide aqueous solution (aluminum oxide aqueous solution massfraction is 1.5%～2.5%) to clean, adopt the concrete steps of aluminum oxide aqueous cleaning to be: a silk is layered on glass, the aluminum oxide aqueous solution configuring is dropped on silk, Graphite Electrodes is polished in the direction of the clock, adopt afterwards deionized water rinsing to fall Graphite Electrodes spot.
2) modification of solid electrode:
Getting appropriate c, to be added drop-wise to chitosan solution (compound method of chitosan solution is: take 0.04g chitosan and be diluted to 3.8ml with the acetic acid of 1% volume fraction) inner, after mixing, absorption drips on the Graphite Electrodes of handling well, dries the Graphite Electrodes (or drying with infrared lamp) of modified.
3) test:
Using the Graphite Electrodes of modified as working electrode, platinum electrode is as supporting electrode, Hg 2cl 2as reference electrode, be placed in electrolyzer, electrolytic solution is that (compound method of electrolytic solution is molecular gel electrolyte: the carbonic allyl ester solution of first preparing lithium perchlorate, the concentration of lithium perchlorate is 0.15mol, then get lithium perchlorate carbonic allyl ester solution 4.06g, add 0.126g gelator water, the content of gelator water in solution is 0.04mol), the parameter of cyclic voltammetry is set to: initial potential is 0.5V, switch current potential 1 is 0.5V, switch current potential 2 is-0.5V, sweep velocity is 0.1V/S, cycle index is 100 times, by cyclic voltammetry, test and obtain Fig. 9, the cyclic voltammetric of c as seen from Figure 9, at 100 redox peaks of circulation, substantially can not change.
It is main raw material Hydrothermal Synthesis MoO that the present invention selects ammonium molybdate 2, by the cyclic voltammetric in x-ray powder instrument, transmission scanning electron microscope, infrared, fluorescence, electrochemical workstation, investigate it and form structure and optical and electrical properties, take potassium bichromate or tropeolin-D as model pollutant research MoO 2absorption property and photocatalytic activity, learn:
1, the MoO making by the method for the invention 2cyclic voltammetric is functional, can be used for the exploitation of lithium ion battery;
2, the MoO making by the method for the invention 2absorption property under closed black dark condition, the photocatalytic activity under tungsten lamp or fluorescent lamp are all best, can be used for semiconductor light-catalyst and process water pollutant.
By drawing above: the MoO that adopts the method for the invention to obtain 2the nano composite material of preparation has vast potential for future development to the field of the processing in sewage field and lithium cell exploitation aspect.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all improvement and conversion all should belong to the protection domain of claims of the present invention.

Claims (4)

1. a MoO with good photoelectric properties 2the preparation method of powder, is characterized in that, comprises the following steps:
S10: the ammonium molybdate aqueous solution that compound concentration is 25mg/L;
S20: add acetic acid and glucose in ammonium molybdate solution, and stir, obtain the solution mixing;
S30: step S20 gained solution is sealed in reactor and is heated, make it carry out reduction reaction, obtain throw out;
S40: adopt reagent to carry out filtering and washing processing step S30 gained throw out, obtain brownish black precipitation;
S50: step S40 gained brownish black precipitation is carried out to drying treatment, grind and obtain MoO 2powder;
Described MoO 2powder is prepared from according to 1g ammonium molybdate proportioning 34ml deionized water, 4ml acetic acid, 1g glucose.
2. the MoO with good photoelectric properties according to claim 1 2the preparation method of powder, is characterized in that, the reduction reaction that described step S30 occurs is carried out in the stainless steel cauldron of poly-four vinyl liner.
3. the MoO with good photoelectric properties according to claim 1 2the preparation method of powder, is characterized in that, in described step S40, suction filtration is processed and comprised:
A: adopt deionized water lotion 4-6 time;
B: adopt dehydrated alcohol lotion 1-2 time.
4. one kind according to the arbitrary described MoO with good photoelectric properties of claim 1-3 2the application of the preparation method of powder in preparing sorbing material and semiconductor light-catalyst.
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CN106177952A (en) * 2016-08-26 2016-12-07 广西师范大学 There is the preparation method and its usage of the molybdenum oxide nanoparticle of targeting photo-thermal, optical dynamic therapy function
CN108054283A (en) * 2017-12-14 2018-05-18 中国科学院化学研究所 A kind of insensitive molybdenum trioxide anode interface layer of film thickness and preparation method thereof and the application in organic solar batteries
CN108940259A (en) * 2018-03-21 2018-12-07 中国矿业大学 A kind of porous MoO of hierarchical structure2Photochemical catalyst microballoon and preparation method thereof
CN110302740A (en) * 2019-07-08 2019-10-08 南昌航空大学 A kind of preparation method and applications of unformed molybdenum oxide adsorbent material
CN112195483A (en) * 2020-09-22 2021-01-08 深圳先进技术研究院 Method for constructing Z-type heterojunction photo-anode and Z-type heterojunction photo-anode
CN112371119A (en) * 2020-11-13 2021-02-19 中南大学深圳研究院 Preparation method and application of multi-metal paired alkaline catalyst

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106177952A (en) * 2016-08-26 2016-12-07 广西师范大学 There is the preparation method and its usage of the molybdenum oxide nanoparticle of targeting photo-thermal, optical dynamic therapy function
CN106177952B (en) * 2016-08-26 2019-12-27 广西师范大学 Preparation method and application of molybdenum oxide nanoparticles with targeted photothermal and photodynamic therapy functions
CN108054283A (en) * 2017-12-14 2018-05-18 中国科学院化学研究所 A kind of insensitive molybdenum trioxide anode interface layer of film thickness and preparation method thereof and the application in organic solar batteries
CN108940259A (en) * 2018-03-21 2018-12-07 中国矿业大学 A kind of porous MoO of hierarchical structure2Photochemical catalyst microballoon and preparation method thereof
CN108940259B (en) * 2018-03-21 2020-07-31 中国矿业大学 Hierarchical porous MoO2Photocatalyst microsphere and preparation method thereof
CN110302740A (en) * 2019-07-08 2019-10-08 南昌航空大学 A kind of preparation method and applications of unformed molybdenum oxide adsorbent material
CN110302740B (en) * 2019-07-08 2021-07-09 南昌航空大学 Application of amorphous molybdenum oxide adsorption material
US11767237B2 (en) 2019-07-08 2023-09-26 Nanchang Hangkong University Method for preparing amorphous molybdenum oxide adsorption material and application thereof
CN112195483A (en) * 2020-09-22 2021-01-08 深圳先进技术研究院 Method for constructing Z-type heterojunction photo-anode and Z-type heterojunction photo-anode
CN112195483B (en) * 2020-09-22 2021-11-16 深圳先进技术研究院 Method for constructing Z-type heterojunction photo-anode and Z-type heterojunction photo-anode
CN112371119A (en) * 2020-11-13 2021-02-19 中南大学深圳研究院 Preparation method and application of multi-metal paired alkaline catalyst
CN112371119B (en) * 2020-11-13 2023-07-07 中南大学深圳研究院 Preparation method and application of multi-metal pairing alkaline catalyst

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