CN106006718B - A kind of zinc sulphide, cuprous sulfide and carbon nano-composite material and preparation method thereof - Google Patents

A kind of zinc sulphide, cuprous sulfide and carbon nano-composite material and preparation method thereof Download PDF

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CN106006718B
CN106006718B CN201610311071.2A CN201610311071A CN106006718B CN 106006718 B CN106006718 B CN 106006718B CN 201610311071 A CN201610311071 A CN 201610311071A CN 106006718 B CN106006718 B CN 106006718B
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zinc
copper
benzoate
zinc sulphide
cuprous sulfide
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CN106006718A (en
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王连英
王东阳
刘改利
魏博文
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/08—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of one-dimensional zinc sulphide, cuprous sulfide and carbon nano-composite materials and preparation method thereof.The present invention is using zinc salt, mantoquita and benzoate as raw material, utilize the coordination of the carboxyl functional group of zinc ion, copper ion and benzoate anion, self assembly has obtained benzoate anion intercalation stratiform hydroxide zinc-copper nanocomposite in aqueous phase solution, again with the benzoate anion intercalation stratiform zinc hydroxide nanocomposite by with stink damp precursor reactant, products therefrom is calcined in nitrogen is made zinc sulphide, cuprous sulfide and carbon nano-composite material.Preparation process of the present invention is simple, and raw material sources are abundant, and production is easy to amplify, and the Effective Regulation of the compound and cuprous sulfide nano-particles size and dispersibility of cuprous sulfide, zinc sulphide and carbon nanomaterial is realized by solid-state method for pyrolysis.

Description

A kind of zinc sulphide, cuprous sulfide and carbon nano-composite material and preparation method thereof
Technical field
The invention belongs to semiconductor nanometer composite material preparing technical fields, and in particular to a kind of zinc sulphide, cuprous sulfide With carbon nano-composite material and preparation method thereof.
Background technology
Nanometer ZnS is a kind of important II-VI group wide band gap semiconducter, has photo-generate electron-hole speed fast and electronics The negative feature of reduction potential height.ZnS belong to broad stopband photochemical catalyst can only by ultraviolet excitation, and in sunlight this portion of energy compared with It is low.Cu2S is a kind of p-type narrowband based semiconductor material, and energy gap about 1.2ev can be had good by excited by visible light Chemically and thermally stability has huge applications potential planting good photocatalysis field.Utilize Cu2S, which is modified ZnS, becomes light The hot spot of catalytic field.Robin Jude, Vimal Michael etc. use solvent-thermal method dodecyl sodium sulfate, zinc acetate Cu is prepared with the mixed liquor of copper acetate2S/ZnS nanocomposites, Thelma Serrano etc. are used using colloid liquid-phase growth method The PbS/Cu of 3- mercaptopropionic acids and trisodium citrate as stabilizer synthesis core shell structure2S/ZnS nanocomposites.But it is above-mentioned Cu in document2The synthetic method of S usually requires Cu (I) precursor, organic solvent, surfactant, undoubtedly increases cost, is not so good as Fabricated in situ is economical and practical, and is easy to pollute the environment.
In recent years, semiconductor-carbon nano-composite material is produced as photochemical catalyst in degradable organic pollutant and photocatalytic water H2Field is widely used.Utilize graphene, CNT and the higher carbon sp of CNF2Hydridization and the big plane π-pi-conjugated structure of two dimension, with half Conductor catalyst combine after, graphene, CNT and CNF can speed up as electron acceptor the light induced electron of semiconductor, hole divide From to improve the photocatalytic activity of semiconductor.
Layered composite metal hydroxides chemical composition is [M2+ 1-xM3+ x(OH)2](An-)x/n·mH2O, laminate metal height Disperse and covalently combine, there are electrostatic force, hydrogen bond and Van der Waals forces with laminate for interlayer guest molecule, and orderly arrange Row form supramolecular structure composite material.It tends to obtain structural homogeneity using layered composite metal hydroxides as presoma The excellent catalyst material of energy.
Invention content
The present invention provides a kind of one-dimensional zinc sulphide, cuprous sulfide and carbon nano-composite materials and preparation method thereof.
The present invention utilizes the carboxyl official of zinc ion, copper ion and benzoate anion using zinc salt, mantoquita and benzoate as raw material Can group coordination, in aqueous phase solution self assembly obtained the nano combined material of benzoate anion intercalation stratiform hydroxide zinc-copper Material, then with the benzoate anion intercalation stratiform zinc hydroxide nanocomposite by with stink damp precursor reactant, products therefrom exists It is calcined in nitrogen and zinc sulphide, cuprous sulfide and carbon nano-composite material is made.
The preparation method of zinc sulphide of the present invention, cuprous sulfide and carbon nano-composite material, is as follows：
1) it is 0.01-1molL by total concentration-1Inorganic zinc salt and copper salt solution and a concentration of 0.01-2molL-1Benzoate aqueous solution uniformly mixed in four-hole bottle, wherein the molar ratio of zinc ion and copper ion be 1:1-6:1, it is inorganic The molar ratio of zinc salt and benzoate is 5:1-1:5；
2) use NaOH solution regulating step 1) prepare mixing salt solution pH value be 5-7, reacted at 25-100 DEG C 0.5-48 hours, product spent CO2Deionized water centrifuge washing, it is dry, obtain benzoate anion intercalation layered hydroxide forerunner Body；
3) benzoate anion intercalation layered hydroxide presoma made from step 2) is positioned in wide-mouth bottle, with 5- 100mL·min-1Flow velocity H is passed through into bottle2S gas reactions 1-60 minutes obtain zinc sulphide, vulcanization copper solid solution and benzene first Sour nanocomposite；
4) by zinc sulphide made from step 3), vulcanization copper solid solution and benzoic acid nanocomposite in 450-700 DEG C of nitrogen 0.5-8h is calcined under gas atmosphere, obtains zinc sulphide, cuprous sulfide and carbon nano-composite material.
Inorganic zinc salt described in step 1) is selected from one or more of zinc nitrate, zinc chloride, zinc sulfate.
Inorganic mantoquita described in step 1) is selected from one or more of copper nitrate, copper chloride, copper sulphate.
Benzoate described in step 1) is one or both of sodium benzoate, Potassium Benzoate.
The concentration range of NaOH solution is 0.1-2molL in step 2)-1。
Reaction temperature is 20-80 DEG C in step 3).
Compared with the prior art, the advantages of the present invention are as follows：Using in benzoate anion intercalation layered hydroxide presoma It is sub- to be pyrolyzed to obtain vulcanization using solid phase in situ for the evenly dispersed feature of laminate metallic zinc copper ion atomic level and carbon material effect The composite material of copper, zinc sulphide and carbon realizes sub- to zinc sulphide vulcanization in zinc sulphide, cuprous sulfide and carbon nano-composite material Effective control of copper nano-particle size and dispersibility；Cuprous sulfide is narrowband based semiconductor, can be in visible-range effectively Promotion zinc sulphide cuprous sulfide nano-particle and carbon between electrons and holes detach, improve catalytic efficiency；The present invention prepares work Skill is simple, and raw material sources are abundant, and production is easy to amplify；The zinc sulphide of quantum size, cuprous sulfide nano-particle are realized in carbon It is evenly dispersed in substrate, enhance the stability of catalyst.
Description of the drawings
Fig. 1 be embodiment 1 prepare benzoate anion intercalation stratiform zinc hydroxide copper precursors (a), zinc sulphide copper solid solution with The X-ray of gained zinc sulphide, cuprous sulfide and carbon nano-composite material (c) is brilliant after benzoic acid nanocomposite (b) and calcining Body diffracting spectrum (XRD).
Fig. 2 is the raman spectrum of the zinc sulphide of the preparation of embodiment 1, cuprous sulfide and carbon nano-composite material.
Fig. 3 is the stereoscan photograph of the zinc sulphide of the preparation of embodiment 1, cuprous sulfide and carbon nano-composite material.
Fig. 4 is that the high-resolution-ration transmission electric-lens of zinc sulphide, cuprous sulfide and carbon nano-composite material prepared by embodiment 1 shine Piece.
Specific implementation mode
Preparation method of the present invention is described further with reference to specific embodiment, but the guarantor of the present invention Shield range is not limited to this.
Embodiment 1
Prepare the mixing salt solution of zinc nitrate and copper nitrate, wherein Zn2+A concentration of 0.08M, Cu2+A concentration of 0.02M； Compound concentration is the PhCOONa solution of 0.03M；Above two solution is added in four-hole bottle simultaneously, sodium benzoate and zinc nitrate Molar ratio be 2, take 0.5M sodium hydroxide solution adjust pH value be 6.2, keep reaction temperature be 80 DEG C, crystallization for 24 hours after, wash It washs, low temperature drying；By the presoma of preparation H at room temperature2It is reacted 1 minute in S atmosphere, H2S gas flow rates are 100mLmin-1, zinc sulphide, copper sulfide and benzoic acid nanocomposite are obtained, then by zinc sulphide, copper sulfide and benzoic acid composite Nano material Expect that roasting 8h in a nitrogen atmosphere in 650 DEG C obtains zinc sulphide, cuprous sulfide and carbon nano-composite material.
Benzoate anion intercalation stratiform hydroxide zinc-copper, which is can be seen that, from Fig. 1-a in low 2 θ angular regions stratiform hydrogen-oxygen occurs The distinctive stratiform peak (00l) of compound, these diffraction peak intensities are high, half-peak width illustrates that the nanofiber crystallinity of synthesis is high.Spread out It penetrates peak and corresponds respectively to presoma (001), (002), (003) diffraction maximum, 2 angles θ corresponding to diffraction maximum are respectively 6.02 °, 11.82 ° and 17.68 ° corresponding interlamellar spacings are 1.46nm, 0.74nm and 5.01nm.Good multiple proportion is presented, illustrates to close At precursor be layer structure.It can be seen that from Fig. 1-b and be passed through H2After S gases, precursor peaks disappearance occur benzoic acid and cube The diffraction maximum of crystalline phase zinc sulphide.It can be seen that zinc sulphide copper solid solution with benzoic acid nanocomposite after calcining from Fig. 1-c There is apparent ZnS and Cu2S diffraction maximums.
Figure it is seen that zinc sulphide, cuprous sulfide, carbon nano-composite material sample are in 1334cm-1The broad peak at place is stone The black peaks carbon characteristic peak D are the disordered structure of graphitic carbon.Sample is in 1594cm-1The peak type point and a height of graphitic carbon feature of intensity at place The peak peaks G, the degree of graphitization of carbon structural nano is usually by the intensity at the peaks D and the peaks G ratio ID/IGIt indicates, herein ID/IGValue is 0.81, Less than 1, illustrate the Zn prepared1-xCu2xCelion in S/C nanofibers has very high degree of graphitization.
Zinc sulphide, cuprous sulfide, the carbon nano-composite material pattern prepared as can be seen from Figure 3 is uniform nanofiber Shape, length are some tens of pm, and diameter is between 150-200nm.
The interlamellar spacing of lattice fringe is 0.31nm as seen from Figure 4 and the interlamellar spacing of lattice fringe is receiving for 0.198nm Rice corpuscles is wrapped in carbon substrate, and the interlamellar spacing of lattice fringe is 0.31nm and (111) diffraction maximum of cubic phase zinc sulphide Interplanar distance numerical value is consistent, and the interlamellar spacing of lattice fringe is the interplanar distance number of (110) diffraction maximum of 0.198nm and cuprous sulfide Value is consistent, and Zinc sulfide nano-particle grain size is about 15nm, and cuprous sulfide nano particle diameter is about 10nm.
Embodiment 2
Prepare the mixing salt solution of zinc nitrate and copper nitrate, a concentration of 0.05M of wherein Zn2+, a concentration of 0.05M of Cu2+； Compound concentration is the PhCOONa solution of 0.05M；Above two solution is added in four-hole bottle simultaneously, sodium salicylate and zinc nitrate Molar ratio be 0.5, by above two solution simultaneously be added in four-hole bottle, take 0.5M sodium hydroxide solution adjust pH value be 7, It is 80 DEG C to keep reaction temperature, crystallization for 24 hours after, washing, low temperature drying will be anti-in the presoma of preparation at room temperature H2S atmosphere It answers 60 minutes, obtains zinc sulphide, copper sulfide and benzoic acid composite nano materials, then answer zinc sulphide, copper sulfide and benzoic acid Conjunction nano material roasts 8h in 650 DEG C and obtains zinc sulphide, cuprous sulfide and carbon nano-composite material in a nitrogen atmosphere.

Claims (1)

1. the preparation method of a kind of zinc sulphide, cuprous sulfide and carbon nano-composite material, which is characterized in that its specific steps is such as Under：
1) it is 0.01-1molL by total concentration-1Inorganic zinc salt and copper salt solution and a concentration of 0.01-2molL-1Benzene Formic acid saline solution uniformly mixes in four-hole bottle, and wherein the molar ratio of zinc ion and copper ion is 1:1-6:1, inorganic zinc salt and The molar ratio of benzoate is 5:1-1:5；
2) use NaOH solution regulating step 1) prepare mixing salt solution pH value be 5-7, react 0.5- at 25-100 DEG C 48 hours, product spent CO2Deionized water centrifuge washing, it is dry, obtain benzoate anion intercalation layered hydroxide presoma；
3) benzoate anion intercalation layered hydroxide presoma made from step 2) is positioned in wide-mouth bottle, with 5-100mL min-1Flow velocity H is passed through into bottle2It is multiple to obtain zinc sulphide, vulcanization copper solid solution and benzoic acid nanometer for S gas reactions 1-60 minutes Condensation material；
4) by zinc sulphide made from step 3), vulcanization copper solid solution and benzoic acid nanocomposite in 450-700 DEG C of nitrogen gas 0.5-8h is calcined under atmosphere, obtains zinc sulphide, cuprous sulfide and carbon nano-composite material；
Inorganic zinc salt described in step 1) is selected from one or more of zinc nitrate, zinc chloride, zinc sulfate；
Inorganic mantoquita described in step 1) is selected from one or more of copper nitrate, copper chloride, copper sulphate；
Benzoate described in step 1) is one or both of sodium benzoate, Potassium Benzoate；
The concentration range of NaOH solution is 0.1-2molL in step 2)-1；
Reaction temperature is 20-80 DEG C in step 3).
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CN108649082B (en) * 2018-04-18 2020-01-17 南京信息工程大学 ZnS carbon quantum dot solar blind ultraviolet detector and preparation method thereof
CN109384223A (en) * 2018-09-07 2019-02-26 北京理工大学 A kind of preparation of the derivative porous carbon electrodes of inorganic salts
CN110526276A (en) * 2019-08-19 2019-12-03 上海大学 A kind of preparation method and its air-sensitive application of ultra-thin Zinc oxide nano sheet
CN112679800B (en) * 2020-12-28 2022-05-13 湖北工业大学 Preparation method and application of asphalt aging-resistant material

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