CN106006718A - Zinc-sulfide, cuprous-sulfide and carbon nanocomposite and preparing method thereof - Google Patents

Zinc-sulfide, cuprous-sulfide and carbon nanocomposite and preparing method thereof Download PDF

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CN106006718A
CN106006718A CN201610311071.2A CN201610311071A CN106006718A CN 106006718 A CN106006718 A CN 106006718A CN 201610311071 A CN201610311071 A CN 201610311071A CN 106006718 A CN106006718 A CN 106006718A
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sulfide
zinc
copper
cuprous
salt
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CN106006718B (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 one-dimensional zinc-sulfide, cuprous-sulfide and carbon nanocomposite and a preparing method thereof. The preparing method includes the steps that zinc salt, copper salt and benzoate serve as raw materials, the coordination of zinc ions, copper ions and carboxyl functional groups of benzoic acid radicals is adopted, self assembling is carried out in an aqueous phase solution, and a benzoic-acid-radical-intercalation layered zinc-hydroxide-copper nanocomposite is obtained; then the benzoic-acid-radical-intercalation layered zinc-hydroxide-copper nanocomposite is reacted with hydrogen sulfide, the product is roasted in nitrogen, and the zinc-sulfide, cuprous-sulfide and carbon nanocomposite is prepared. According to the zinc-sulfide, cuprous-sulfide and carbon nanocomposite and the preparing method, the preparing technology is simple, sources of raw materials are rich, production is easy to enlarge, and compounding of cuprous sulfide, zinc sulfide and carbon nanomaterials and effective regulating and control of the size and the dispersity of cuprous sulfide nano particles are achieved with a solid-state pyrolysis method.

Description

A kind of zinc sulfide, cuprous sulfide and carbon nano-composite material and preparation method thereof
Technical field
The invention belongs to semiconductor nanometer composite material preparing technical field, be specifically related to a kind of zinc sulfide, sulfuration Cuprous and 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 electric The feature that sub-reduction potential height is negative.ZnS belong to broad stopband photocatalyst can only by ultraviolet excitation, and in sunlight this Portion of energy is relatively low.Cu2S is a kind of p-type arrowband based semiconductor material, energy gap about 1.2ev, it is possible to quilt can See that light excites, there is good chemically and thermally stability have huge applications to dive planting good photocatalysis field Energy.Utilize Cu2S becomes the focus of photocatalysis field to ZnS modification.Robin Jude、Vimal Michael Cu is prepared Deng the mixed liquor using solvent-thermal method dodecyl sodium sulfate, zinc acetate and copper acetate2S/ZnS nanometer Composite, Thelma Serrano etc. uses colloid liquid-phase growth method 3-mercaptopropionic acid and trisodium citrate conduct The PbS/Cu of stabilizer synthetic kernel shell structure2S/ZnS nano composite material.But Cu in above-mentioned document2The synthesis of S Method typically requires Cu (I) precursor, organic solvent, surfactant, adds cost undoubtedly, not as closing in situ Become economical and practical, and easily to environment.
In recent years, quasiconductor-carbon nano-composite material as photocatalyst in degradable organic pollutant and photocatalytic water system Take H2Field is widely used.Utilize the carbon sp that Graphene, CNT and CNF are higher2Hydridization and two dimension big plane π-π Conjugated structure, after being combined with semiconductor catalyst, Graphene, CNT and CNF can speed up as electron acceptor The light induced electron of quasiconductor, the separation in hole, thus improve the photocatalytic activity of quasiconductor.
Layered composite metal hydroxides chemical composition is [M2+ 1-xM3+ x(OH)2](An-)x/n·mH2O, laminate metal High degree of dispersion also covalently combines, and interlayer guest molecule and laminate exist electrostatic force, hydrogen bond and model moral Hua Li, and ordered arrangement formation supramolecular structure composite.Using layered composite metal hydroxides as forerunner Body tends to obtain the catalyst material that even structure performance is excellent.
Summary of the invention
The invention provides a kind of one-dimensional zinc sulfide, cuprous sulfide and carbon nano-composite material and preparation method thereof.
The present invention, with zinc salt, mantoquita and benzoate as raw material, utilizes zinc ion, copper ion and benzoate anion The coordination of carboxyl functional group, in aqueous phase solution, self assembly has obtained benzoate anion intercalation stratiform zinc hydroxide Copper nano composite material, then with this benzoate anion intercalation stratiform zinc hydroxide nano composite material by with hydrogen sulfide Gas reaction, products therefrom is calcined in nitrogen and is prepared zinc sulfide, cuprous sulfide and carbon nano-composite material.
Zinc sulfide of the present invention, cuprous sulfide and the preparation method of carbon nano-composite material, concrete steps are such as Under:
1) it is 0.01-1mol L by total concentration-1Inorganic zinc salt and copper salt solution, and concentration is 0.01-2mol L-1 Benzoate aqueous solution uniformly mix in four-hole bottle, wherein the mol ratio of zinc ion and copper ion is 1:1-6:1, The mol ratio of inorganic zinc salt and benzoate is 5:1-1:5；
2) NaOH solution regulating step 1 is used) pH value of mixing salt solution prepared is 5-7, at 25-100 DEG C Lower reaction 0.5-48 hour, product spends CO2Deionized water centrifuge washing, is dried, obtains benzoate anion intercalation Layered hydroxide presoma；
3) by step 2) prepare benzoate anion intercalation layered hydroxide presoma be positioned in wide mouthed bottle, with 5-100mL·min-1Flow velocity in bottle, be passed through H2S gas reaction 1-60 minute, obtains zinc sulfide, copper sulfide Solid solution and benzoic acid nano composite material；
4) by step 3) zinc sulfide for preparing, copper sulfide solid solution and benzoic acid nano composite material be in 450-700 DEG C Calcine 0.5-8h under nitrogen atmosphere, obtain zinc sulfide, cuprous sulfide and carbon nano-composite material.
Step 1) described in one or more in zinc nitrate, zinc chloride, the zinc sulfate of inorganic zinc salt.
Step 1) described in one or more in copper nitrate, copper chloride, the copper sulfate of inorganic mantoquita.
Step 1) described in benzoate be one or both in sodium benzoate, Potassium Benzoate.
Step 2) in the concentration range of NaOH solution be 0.1-2mol L-1。
Step 3) in reaction temperature be 20-80 DEG C.
Compared with prior art, it is an advantage of the current invention that: utilize benzoate anion intercalation layered hydroxide forerunner The body la m metallic zinc homodisperse feature of copper ion atomic level and material with carbon element effect, use solid-phase thermal in situ Solution obtains the composite of cuprous sulfide, zinc sulfide and carbon, it is achieved that to zinc sulfide, cuprous sulfide and carbon nanometer Zinc sulfide cuprous sulfide nano-particles size and effective control of dispersibility in composite；Cuprous sulfide is arrowband Based semiconductor, can be effectively promoted electronics between zinc sulfide cuprous sulfide nanoparticle and carbon in visible-range Separate with hole, improve catalytic efficiency；Preparation technology of the present invention is simple, abundant raw material source, produces and is prone to put Greatly；Achieve dispersed in carbon substrate of the zinc sulfide of quantum size, cuprous sulfide nanoparticle, strengthen The stability of catalyst.
Accompanying drawing explanation
Fig. 1 is benzoate anion intercalation stratiform zinc hydroxide copper precursors (a) of embodiment 1 preparation, sulfuration zinc-copper solid solution Gained zinc sulfide, cuprous sulfide and carbon nano-composite material (c) after body and benzoic acid nano composite material (b) and calcining X-ray crystal diffraction collection of illustrative plates (XRD).
Fig. 2 is the Raman spectrogram of the zinc sulfide of embodiment 1 preparation, cuprous sulfide and carbon nano-composite material.
Fig. 3 is the stereoscan photograph of the zinc sulfide of embodiment 1 preparation, cuprous sulfide and carbon nano-composite material.
Fig. 4 is that the zinc sulfide of embodiment 1 preparation, cuprous sulfide are electric with the high-resolution transmission of carbon nano-composite material Mirror photo.
Detailed description of the invention
Below in conjunction with specific embodiment, preparation method of the present invention is described further, but the present invention Protection domain be not limited to this.
Embodiment 1
Preparation zinc nitrate and the mixing salt solution of copper nitrate, wherein Zn2+Concentration be 0.08M, Cu2+Concentration is 0.02M；Compound concentration is the PhCOONa solution of 0.03M；Above two solution is simultaneously introduced in four-hole bottle, Sodium benzoate is 2 with the mol ratio of zinc nitrate, and the sodium hydroxide solution regulation pH value taking 0.5M is 6.2, keeps Reaction temperature is 80 DEG C, after crystallization 24h, and washing, oven drying at low temperature；Presoma H at room temperature by preparation2S Atmosphere is reacted 1 minute, H2S gas flow rate is 100mL min-1, obtain zinc sulfide, copper sulfide and benzoic acid Nano composite material, then by zinc sulfide, copper sulfide and benzoic acid composite nano materials in 650 DEG C at nitrogen atmosphere Lower roasting 8h obtains zinc sulfide, cuprous sulfide and carbon nano-composite material.
From Fig. 1-a it can be seen that benzoate anion intercalation stratiform hydroxide zinc-copper stratiform occurs in low 2 θ angle ranges Hydroxide distinctive stratiform peak (00l), these diffraction peak intensities are high, the nanofiber of half-peak width explanation synthesis Degree of crystallinity is high.Diffraction maximum corresponds respectively to presoma (001), (002), (003) diffraction maximum, corresponding to diffraction maximum Respectively 6.02 ° of 2 θ angles, 11.82 ° and 17.68 ° of corresponding interlamellar spacings are 1.46nm, 0.74nm and 5.01nm. All present good multiple proportion, illustrate that the precursor of synthesis is layer structure.Can be seen that from Fig. 1-b and be passed through H2S After gas, precursor peaks disappears and occurs in that benzoic acid and the diffraction maximum of cube crystalline phase zinc sulfide.Can be seen that from Fig. 1-c Sulfuration zinc-copper solid solution occurs obvious ZnS and Cu with benzoic acid nano composite material after calcining2S diffraction maximum.
Figure it is seen that zinc sulfide, cuprous sulfide, carbon nano-composite material sample are at 1334cm-1Place Broad peak is graphitic carbon characteristic peak D peak, for the disordered structure of graphitic carbon.Sample is at 1594cm-1The peak type point at place and Intensity a height of graphitic carbon characteristic peak G peak, the degree of graphitization of carbon structural nano is generally by D peak and the intensity at G peak Compare ID/IGRepresent, I hereinD/IGValue is 0.81, less than 1, the Zn of preparation is described1-xCu2xIn S/C nanofiber Celion there is the highest degree of graphitization.
The zinc sulfide prepared as can be seen from Figure 3, cuprous sulfide, carbon nano-composite material pattern are for receive uniformly Rice threadiness, a length of some tens of pm, diameter is between 150-200nm.
The interlamellar spacing of lattice fringe is 0.31nm and the interlamellar spacing of lattice fringe is 0.198nm as seen from Figure 4 Nanoparticle be wrapped in carbon substrate, the interlamellar spacing of lattice fringe is 0.31nm and cube crystalline phase zinc sulfide (111) the interplanar distance numerical value of diffraction maximum is consistent, and the interlamellar spacing of lattice fringe is (110) of 0.198nm and cuprous sulfide The interplanar distance numerical value of diffraction maximum is consistent, and Zinc sulfide nano-particle particle diameter is about 15nm, cuprous sulfide nanometer Particle diameter is about 10nm.
Embodiment 2
Preparation zinc nitrate and the mixing salt solution of copper nitrate, wherein the concentration of Zn2+ is that 0.05M, Cu2+ concentration is 0.05M；Compound concentration is the PhCOONa solution of 0.05M；Above two solution is simultaneously introduced in four-hole bottle, Sodium salicylate is 0.5 with the mol ratio of zinc nitrate, is simultaneously introduced in four-hole bottle by above two solution, takes 0.5M Sodium hydroxide solution regulation pH value be 7, keep reaction temperature be 80 DEG C, after crystallization 24h, washing, low temperature Dry, will preparation presoma H2S atmosphere at room temperature in react 60 minutes, obtain zinc sulfide, copper sulfide with Benzoic acid composite nano materials, then by zinc sulfide, copper sulfide and benzoic acid composite nano materials in 650 DEG C at nitrogen Under gas atmosphere, roasting 8h obtains zinc sulfide, cuprous sulfide and carbon nano-composite material.

Claims (6)

1. the preparation method of a zinc sulfide, cuprous sulfide and carbon nano-composite material, it is characterised in that its tool Body step is as follows:
1) it is 0.01-1mol L by total concentration-1Inorganic zinc salt and copper salt solution, and concentration is 0.01-2mol L-1 Benzoate aqueous solution uniformly mix in four-hole bottle, wherein the mol ratio of zinc ion and copper ion is 1:1-6:1, The mol ratio of inorganic zinc salt and benzoate is 5:1-1:5；
2) NaOH solution regulating step 1 is used) pH value of mixing salt solution prepared is 5-7, at 25-100 DEG C Lower reaction 0.5-48 hour, product spends CO2Deionized water centrifuge washing, is dried, obtains benzoate anion intercalation Layered hydroxide presoma；
3) by step 2) prepare benzoate anion intercalation layered hydroxide presoma be positioned in wide mouthed bottle, with 5-100mL·min-1Flow velocity in bottle, be passed through H2S gas reaction 1-60 minute, obtains zinc sulfide, copper sulfide Solid solution and benzoic acid nano composite material；
4) by step 3) zinc sulfide for preparing, copper sulfide solid solution and benzoic acid nano composite material be in 450-700 DEG C Calcine 0.5-8h under nitrogen atmosphere, obtain zinc sulfide, cuprous sulfide and carbon nano-composite material.
Preparation method the most according to claim 1, it is characterised in that step 1) described in inorganic zinc One or more in zinc nitrate, zinc chloride, zinc sulfate of salt.
Preparation method the most according to claim 1, it is characterised in that step 1) described in Inorganic Copper One or more in copper nitrate, copper chloride, copper sulfate of salt.
Preparation method the most according to claim 1, it is characterised in that step 1) described in benzoic acid Salt is one or both in sodium benzoate, Potassium Benzoate.
Preparation method the most according to claim 1, it is characterised in that step 2) in NaOH solution Concentration range is 0.1-2mol L-1.
Preparation method the most according to claim 1, it is characterised in that step 3) in reaction temperature be 20-80℃。
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108649082A (en) * 2018-04-18 2018-10-12 南京信息工程大学 A kind of ZnS carbon quantum dots 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
CN112679800A (en) * 2020-12-28 2021-04-20 湖北工业大学 Preparation method and application of asphalt aging-resistant material

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CN103191783A (en) * 2013-04-18 2013-07-10 北京化工大学 Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof
CN104801303A (en) * 2015-05-07 2015-07-29 北京化工大学 Copper/carbon nano composite catalyst and preparation method thereof

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EP1231254A1 (en) * 2001-02-07 2002-08-14 Agfa-Gevaert Preparation of ZnS particles doped with copper
CN102923669A (en) * 2012-11-15 2013-02-13 北京化工大学 Benzoic acid-intercalated laminated transition metal hydroxide one-dimensional nano material with reversible transition structure and preparation method thereof
CN103191783A (en) * 2013-04-18 2013-07-10 北京化工大学 Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof
CN104801303A (en) * 2015-05-07 2015-07-29 北京化工大学 Copper/carbon nano composite catalyst and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108649082A (en) * 2018-04-18 2018-10-12 南京信息工程大学 A kind of ZnS carbon quantum dots 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
CN112679800A (en) * 2020-12-28 2021-04-20 湖北工业大学 Preparation method and application of asphalt aging-resistant material

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