CN105836715B - Controllable self assembly ternary sulphur selenizing molybdenum nanotube of a kind of component and preparation method thereof - Google Patents

Controllable self assembly ternary sulphur selenizing molybdenum nanotube of a kind of component and preparation method thereof Download PDF

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CN105836715B
CN105836715B CN201610185864.4A CN201610185864A CN105836715B CN 105836715 B CN105836715 B CN 105836715B CN 201610185864 A CN201610185864 A CN 201610185864A CN 105836715 B CN105836715 B CN 105836715B
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nanotube
molybdenum
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CN105836715A (en
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许俊
蒋淼
吴梅惠
史正添
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Hefei University of Technology
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    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01B19/00—Selenium; Tellurium; Compounds thereof
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Abstract

The invention discloses controllable self assembly ternary sulphur selenizing molybdenum nanotube of a kind of component and preparation method thereof, it is characterised in that：Sulphur selenizing molybdenum nanotube chemistry formula is Mo (SxSe1‑x)2, it is by layer structure Mo (SxSe1‑x)2Nanometer sheet assembles what is formed, simple low temperature solution polycondensation synthesis of carbon/molybdenum disulfide self assembly pipe is used during preparation, then selenization technology is used, make molybdenum disulfide nano tube selenizing, and regulate and control S/Se atomic ratios in sulphur selenizing molybdenum nanotube by changing selenizing temperature, prepare the controllable ternary sulphur selenizing molybdenum self-assembled nanometer pipe of component.Present invention process is simple, is adapted to large-scale production, can prepare the controllable hexagonal crystal system M o (S of componentxSe1‑x)2Self-assembled nanometer pipe, it is Mo (SxSe1‑x)2Nanotube is laid a good foundation in the application of electrochemical energy storage, electrocatalytic hydrogen evolution and new energy field.

Description

Controllable self assembly ternary sulphur selenizing molybdenum nanotube of a kind of component and preparation method thereof
Technical field
The present invention relates to a kind of self assembly ternary sulphur selenizing molybdenum nanotube Mo (SxSe1-x)2The preparation method of (0≤x≤1), Belong to technical field of nano material.
Background technology
Layer structure Transition-metal dichalcogenide nano structural material is a kind of important semi-conducting material, optics, The fields such as electricity, photoelectric device, electro-catalysis and energy storage device are with a wide range of applications.But such semi-conducting material is ground Study carefully and still concentrate on binary system, to ternary alloy three-partalloy phase metal chalcogenide compound material such as Mo (SxSe1-x)2、W(SxSe1-x)2Etc. grinding Study carefully very few.Ternary alloy three-partalloy phase semiconductor is a kind of novel semi-conducting material, the advantages of can either inheriting parent binary material, again With a series of unique physics and chemical characteristic.Molybdenum category chalcogenide has good Environmental compatibility, nontoxicity, reserves The advantages that abundant.Except passing through quantum size effect, ternary sulphur selenizing molybdenum nano material, additionally it is possible to provide a kind of novel side Formula, i.e. composition regulate and control, and to change the level structure of material, optically and electrically carrier type, characteristic and chemical property etc., realize Function nano device performance regulation and control and optimization, make its in fields such as novel microelectronic device, photoelectric device and energy storage devices all There is important application potential.But the synthesis of ternary alloy three-partalloy phase nano structural material is present that component is uneven, large area prepare it is tired Difficult, easy the problems such as containing binary impurities phase.Therefore explore a kind of simple method and prepare the regulatable ternary sulphur selenizing molybdenum of component Nanotube has important research value and practical application meaning.
The content of the invention
The present invention is to avoid the weak point present in above-mentioned prior art, there is provided a kind of self assembly component it is controllable three First sulphur selenizing molybdenum nanotube and preparation method thereof.
The present invention solves technical problem and adopted the following technical scheme that：
The self assembly ternary sulphur selenizing molybdenum nanotube of the present invention, its feature are：The ternary sulphur selenizing molybdenum nanotube Formula is Mo (SxSe1-x)2, component can regulate and control in the range of 0≤x≤1；Nanotube is by layer structure Mo (SxSe1-x)2Receive Rice piece assembles what is formed；Mo(SxSe1-x)2Tetravalence is presented in middle molybdenum ion；By regulating and controlling Mo (SxSe1-x)2Middle x values, can change it Crystal interlamellar spacing, and effectively improve characteristic of semiconductor, photoelectric properties and the chemical property of material.
The preparation method of the controllable self assembly ternary sulphur selenizing molybdenum nanotube of instant component, is to carry out as follows：
A, 1-5mmol S powder is weighed, is added in 10-100mL n-octyl amine solution, 3-5 minutes are stirred under normal temperature, obtain solution A；
B, 0.5-2.5mmol molybdenum sources are added in the solution A, continues to stir 3-5 minutes under normal temperature, obtains solution B；
C, 10-100mL absolute ethyl alcohols are added in the solution B, obtain mixed solution；The mixed solution is shifted 3-12 hours are reacted into reactor and at 170-200 DEG C, obtain initial product；
D, after the initial product being cleaned and dried, molybdenum disulfide nano tube is obtained；
E, the molybdenum disulfide nano tube is placed in tube furnace, while adds 5-25mmol Se powder, then in argon hydrogen It is warming up under body protection between 700-900 DEG C, is incubated 20-60 minutes, is finally cooled to room temperature, that is, obtains target product self assembly Ternary sulphur selenizing molybdenum nanotube.
Wherein：By changing the reaction temperature in step e, change selenizing degree, so as to goal of regulation and control product Mo (SxSe1-x)2Middle x value, obtain the controllable self assembly ternary sulphur selenizing molybdenum nanotube of component.
The molybdenum source is MoO3Or (NH4)2MoO4。
Cleaning is to use deionized water, watery hydrochloric acid and washes of absolute alcohol successively described in step d.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1st, the invention provides ternary sulphur selenizing molybdenum nanotube and preparation method thereof, products therefrom is in nanotube-shaped, pattern Rule, uniform component, free from admixture phase, electricity and electrochemical properties are excellent；
2nd, preparation method technique of the invention is simple, magnanimity synthesizes, cost is cheap, easy to spread；
3rd, the present invention can regulate and control S/Se atomic ratios in the product sulfur selenizing molybdenum nanotube by selenizing temperature, prepare it is a variety of not It is strong with the sulphur selenizing molybdenum nanotube of component, controllability；
4th, sulphur selenizing molybdenum nanotube prepared by the present invention shows what is extremely protruded as elctro-catalyst in evolving hydrogen reaction Electro catalytic activity, its Hydrogen Evolution Performance are substantially better than binary MoS2And MoSe2。
Brief description of the drawings
Fig. 1 is Mo (S prepared by the embodiment of the present invention 1~4xSe1-x)2The scanning electron microscope diagram of nanotube；
Fig. 2 is Mo (S prepared by the embodiment of the present invention 1~4xSe1-x)2The EDS energy spectrum diagrams of nanotube；
Fig. 3 is Mo (S prepared by the embodiment of the present invention 1~4xSe1-x)2The XRD of nanotube；
Fig. 4 is Mo (S prepared by the embodiment of the present invention 1~4xSe1-x)2The Raman spectrogram of nanotube；
Fig. 5 is as the Mo (S prepared by the embodiment of the present invention 1,3,4xSe1-x)2The electrical performance testing figure of nanotube.
Embodiment
With reference to specific embodiments and the drawings, the present invention will be further described, and is not restricted to the scope of the present invention.
Embodiment 1
The present embodiment prepares Mo (S as followsxSe1-x)2(x=1) nanotube：
A, weigh S powder 1.2mmol (be selected from Shanghai Run Jie chemical reagent Co., Ltd, analysis it is pure (>99.9%)), it is added to In 10mL n-octyl amine solution, stirred 5 minutes under normal temperature, obtain red tan solution A；The beaker glass dish of solution will be placed during stirring Build, carried out in fume hood；
B, 0.5mmol molybdenum trioxides are added in red tan solution A, continues to stir 5 minutes under normal temperature, obtains pale yellow solution B；
C, 15mL absolute ethyl alcohols (analyzing pure AR) are added in pale yellow solution B, obtain mixed solution；By mixed solution It is transferred in reactor at 180 DEG C and reacts 6 hours, obtains initial product；
D, deionized water, watery hydrochloric acid and washes of absolute alcohol initial product are used successively, are then dried 10 hours at 65 DEG C, Molybdenum disulfide nano tube is obtained, is designated as sample 1.
Embodiment 2
The present embodiment prepares Mo (S as followsxSe1-x)2(x=0.84) nanotube：
A, weigh S powder 1.2mmol (be selected from Shanghai Run Jie chemical reagent Co., Ltd, analysis it is pure (>99.9%)), it is added to In 20mL n-octyl amine solution, stirred 5 minutes under normal temperature, obtain red tan solution A；The beaker glass dish of solution will be placed during stirring Build, carried out in fume hood；
B, 0.5mmol molybdenum trioxides are added in red tan solution A, continues to stir 5 minutes under normal temperature, obtains pale yellow solution B；
C, 15mL absolute ethyl alcohols (analyzing pure AR) are added in pale yellow solution B, obtain mixed solution；Mixed solution is turned Move on in reactor and reacted 6 hours at 180 DEG C, obtain initial product；
D, deionized water, watery hydrochloric acid and washes of absolute alcohol initial product are used successively, are then dried 10 hours at 65 DEG C, Obtain molybdenum disulfide nano tube；
E, molybdenum disulfide nano tube is placed in tube furnace, while adds Se powder 5mmol, 700 under the protection of argon hydrogen DEG C heating 1 hour, mix selenium processing, after then naturally cooling to room temperature, that is, obtains sulphur selenizing molybdenum nanotube, be designated as sample 2.
Embodiment 3
The present embodiment prepares Mo (S as followsxSe1-x)2(x=0.22) nanotube：
A, weigh S powder 1.2mmol (be selected from Shanghai Run Jie chemical reagent Co., Ltd, analysis it is pure (>99.9%)), it is added to In 20mL n-octyl amine solution, stirred 5 minutes under normal temperature, obtain red tan solution A；The beaker glass dish of solution will be placed during stirring Build, carried out in fume hood；
B, 0.5mmol molybdenum trioxides are added in red tan solution A, continues to stir 5 minutes under normal temperature, obtains pale yellow solution B；
C, 15mL absolute ethyl alcohols (analyzing pure AR) are added in pale yellow solution B, obtain mixed solution；Mixed solution is turned Move on in reactor and reacted 6 hours at 180 DEG C, obtain initial product；
D, deionized water, watery hydrochloric acid and washes of absolute alcohol initial product are used successively, are then dried 10 hours at 65 DEG C, Obtain molybdenum disulfide nano tube；
E, molybdenum disulfide nano tube is placed in tube furnace, while adds 5mmolSe powder, 800 under the protection of argon hydrogen DEG C heating 1 hour, carry out selenization, after then naturally cooling to room temperature, that is, obtain sulphur selenizing molybdenum nanotube, be designated as sample 3.
Embodiment 4
The present embodiment prepares Mo (S as followsxSe1-x)2(x=0) nanotube：
A, weigh S powder 1.2mmol (be selected from Shanghai Run Jie chemical reagent Co., Ltd, analysis it is pure (>99.9%)), it is added to In 20mL n-octyl amine solution, stirred 5 minutes under normal temperature, obtain red tan solution A；The beaker glass dish of solution will be placed during stirring Build, carried out in fume hood；
B, 0.5mmol molybdenum trioxides are added in red tan solution A, continues to stir 5 minutes under normal temperature, obtains pale yellow solution B；
C, 15mL absolute ethyl alcohols (analyzing pure AR) are added in pale yellow solution B, obtain mixed solution；Mixed solution is turned Move on in reactor and reacted 6 hours at 180 DEG C, obtain initial product；
D, deionized water, watery hydrochloric acid and washes of absolute alcohol initial product are used successively, are then dried 10 hours at 65 DEG C, Obtain molybdenum disulfide nano tube；
E, molybdenum disulfide nano tube is placed in tube furnace, while adds 5mmolSe powder, 900 under the protection of argon hydrogen DEG C heating 1 hour, carry out selenization, after then naturally cooling to room temperature, that is, obtain sulphur selenizing molybdenum nanotube, be designated as sample 4.
Fig. 1 is that the SEM of the gained sample of embodiment 1~4 schemes, a, b, c, d difference counter sample 1, sample 2, sample in Fig. 1 3rd, sample 4, it can be seen that product is all by Mo (SxSe1-x)2Nanometer sheet assembles the hollow nanotube to be formed, and length is about 2-3 μm, Diameter is about 200nm, and with the increase of Se content, the increase of nanotube surface roughness.
Fig. 2 is the EDS energy spectrum diagrams of 1~4 gained sample, shows Mo (SxSe1-x)2In sample 1~4 S contents be respectively x=1, X=0.84, x=0.22 and x=0.
Fig. 3 is the XRD of the gained sample of embodiment 1~4, by being contrasted with standard card, it is known that products therefrom is distinguished Corresponding MoS2(sample 1), ternary Mo (SxSe1-x)2(sample 2, sample 3) and MoSe2(sample 4).As Se content increases, diffraction Peak (110) is offset toward low angle, shows to generate ternary Mo (SxSe1-x)2Nanotube；And (002) crystal face interlamellar spacing is with selenium Change temperature to improve and be substantially reduced.
Fig. 4 is the Raman spectrogram of the gained sample of embodiment 1~4, as seen from the figure as the rising of selenizing temperature is (from sample 700 DEG C of product 2 are gradually increased to 900 DEG C of sample 4), Se contents can also increase in sample.Sample 1 is in 376cm-1And 399cm-1 There are two vibration peaks at place, corresponds to respectivelyAnd A1g(Mo-S)Vibration mode, it is binary MoS to show sample 12.With the phase of sample 1 Than in the Raman spectrum of sample 2 in addition to having the vibration peak from Mo-S keys, in 270cm-1Also there is a vibration peak, it is corresponding A1g(Mo-Se)Vibration mode, it is ternary Mo (S to show sample 2xSe1-x)2.A in sample 31g(Mo-Se)Vibration peak is floated to lower wave number direction Move to 260cm-1, A1g(Mo-S)Vibration peak intensity significantly reduce, show sample 3 and ternary Mo (SxSe1-x)2, but selenium content has Improved.Vibration peak from Mo-S keys in the Raman spectrum of sample 4 has disappeared, and only has A1g(Mo-Se)Vibration peak, and drift about To 234cm-1, it is binary MoSe to show sample 42。
Embodiment 5
To characterize the chemical property of sample obtained by above-described embodiment, make following test.
A, the sample 1 prepared by 1mg, sample 3, sample 4 are dissolved in 125 μ L deionized waters respectively and 125 μ L alcohol (divides Analyse pure AR) mixed solution in, add 5 μ LNafion solution (being selected from Aldrich chemical reagents corporations of the U.S., 5wt%), surpass Sound is uniformly catalyzed solvent in 30 minutes to prepare.
B, 10 μ L catalysis solvents are placed in glass-carbon electrode (electrode jacket diameter 6mm, interior diameter 3mm, long 60mm, selected from day Tianjin Ida Heng Sheng developments in science and technology Co., Ltd) on electrode cores and it is completely covered.It is placed on 60 DEG C of drying bakers to dry 10 minutes, obtains To the uniform catalysis electrode of smearing.
C, (reference fluid 3.5M Klorvess Liquids, ended by the catalysis electrode and saturation Ag/AgCl electrodes that prepare selected from Tianjin Up to Heng Sheng developments in science and technology Co., Ltd), platinum electrode (being selected from Tianjin Aidahengsheng Technology Development Co., Ltd) is respectively as three The working electrode of electrode electric catalyticing system, reference electrode and to electrode, are placed among 5% sulfuric acid solution, carry out electrification Learn collecting gas and determine its chemical property.
D, it is linear using electrochemical workstation (CHI660E electrochemical workstations, selected from Shanghai Chen Hua Instrument Ltd.) Scan the electrocatalytic hydrogen evolution performance of the above-mentioned sample of voltammetry research.
(the binary MoS of derived sample 1 from Fig. 52Nanotube) and (the binary MoSe of sample 42Nanotube) and (the ternary sulphur of sample 3 Selenizing molybdenum nanotube) cathodic polarization curve there were significant differences, ternary sulphur selenizing molybdenum nanotube generates obvious in -0.2V Liberation of hydrogen electric current, show that ternary sulphur selenizing molybdenum nanotube has more preferable electro catalytic activity.

Claims (3)

  1. A kind of 1. preparation method of the controllable self assembly ternary sulphur selenizing molybdenum nanotube of component, it is characterised in that：
    The chemical formula of the ternary sulphur selenizing molybdenum nanotube is Mo (SxSe1-x)2, 0≤x≤1；The ternary sulphur selenizing molybdenum nanotube It is by layer structure Mo (SxSe1-x)2Nanometer sheet assembles to be formed；
    The preparation method of the ternary sulphur selenizing molybdenum nanotube, it is to carry out as follows：
    A, 1-5mmol S powder is weighed, is added in 10-100mL n-octyl amine solution, 3-5 minutes are stirred under normal temperature, obtain solution A；
    B, 0.5-2.5mmol molybdenum sources are added in the solution A, continues to stir 3-5 minutes under normal temperature, obtains solution B；
    C, 10-100mL absolute ethyl alcohols are added in the solution B, obtain mixed solution；The mixed solution is transferred to instead Answer in kettle and reacted 3-12 hours at 170-200 DEG C, obtain initial product；
    D, after the initial product being cleaned and dried, molybdenum disulfide nano tube is obtained；
    E, the molybdenum disulfide nano tube is placed in tube furnace, while adds 5-25mmol Se powder, then in argon hydrogen shield Under be warming up between 700-900 DEG C, be incubated 20-60 minutes, be finally cooled to room temperature, that is, obtain target product self assembly ternary sulphur Selenizing molybdenum nanotube；
    By changing the reaction temperature in step e, so as to goal of regulation and control product Mo (SxSe1-x)2Middle x value, it is controllable to obtain component Self assembly ternary sulphur selenizing molybdenum nanotube.
  2. 2. the preparation method of the controllable self assembly ternary sulphur selenizing molybdenum nanotube of component according to claim 1, its feature It is：The molybdenum source is MoO3Or (NH4)2MoO4·4H2O。
  3. 3. the preparation method of the controllable self assembly ternary sulphur selenizing molybdenum nanotube of component according to claim 1, its feature It is：Cleaning is respectively to be cleaned with deionized water, watery hydrochloric acid and absolute ethyl alcohol successively described in step d.
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CN108585046B (en) * 2018-04-23 2019-10-15 西安交通大学 A kind of high length-diameter ratio molybdenum dioxide nanotube and preparation method thereof
CN108373141B (en) * 2018-05-29 2021-05-18 中国海洋大学 Preparation method of hollow molybdenum selenide sulfide nanospheres
CN111785964B (en) * 2019-04-04 2024-03-22 中南大学 Artificial two-dimensional solid electrolyte interface material of lithium metal battery, anode precursor material, anode, preparation and application thereof
CN110270353A (en) * 2019-04-16 2019-09-24 青岛科技大学 The preparation and application of load transitions bimetallic chalcogen compound nano material in situ
CN110371934B (en) * 2019-06-06 2022-07-22 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） Preparation method of carbon-based sulfur molybdenum selenide composite material
CN110284146A (en) * 2019-06-21 2019-09-27 青岛科技大学 Load selenium in situ adulterates molybdenum disulfide/transition metal boride nano material preparation and application

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