CN104528812A - Preparation method of flower-like PbS/Ni2P composite material - Google Patents

Preparation method of flower-like PbS/Ni2P composite material Download PDF

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Publication number
CN104528812A
CN104528812A CN201410816729.6A CN201410816729A CN104528812A CN 104528812 A CN104528812 A CN 104528812A CN 201410816729 A CN201410816729 A CN 201410816729A CN 104528812 A CN104528812 A CN 104528812A
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flower
pbs
room temperature
add
polytetrafluoroethyllining lining
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CN201410816729.6A
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CN104528812B (en
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刘淑玲
刘慧�
朱建平
仝建波
尤艳雪
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G21/00—Compounds of lead
    • C01G21/21—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/08—Other phosphides
    • 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
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a preparation method of a flower-like PbS/Ni2P composite material. The method comprises the following steps: firstly, preparing uniform flower-like lead sulfide by virtue of a solvothermal method; carrying out hydro-thermal treatment on the flower-like lead sulfide, nickel chloride hexahydrate, a cetyl trimethyl ammonium bromide and lauryl sodium sulfate mixed surfactant and yellow phosphorus at a certain chemical stoichiometric ratio; and drying the obtained product in vacuum, so as to prepare the flower-like PbS/Ni2P composite material. An effective three-dimensional space is provided for nickel phosphide by the flower-like lead sulfide; the technical problem of relatively low catalytic performance caused by agglomeration of nickel phosphide nano-particles is solved; and the method is available in raw material, and simple in preparation method.

Description

A kind of flower-shaped PbS/Ni 2the preparation method of P matrix material
Technical field
The present invention relates to technical field of composite preparation, be specifically related to a kind of flower-shaped PbS/Ni 2the preparation method of P matrix material.
Background technology
Lead sulfide is typical low energy gap based semiconductor, and under room temperature, its energy gap is 0.41eV, and in the past few decades, lead sulfide has been widely used in the aspects such as photoluminescence, opto-electronic conversion, nonlinear optics.Owing to having relatively large Exciton Bohr Radius (18nm), lead sulfide (PbS) is made can quantum size effect to be occurred when larger particle or grain-size.But PbS is unstable, and especially PbS nanoparticle has higher surface energy, and stability is poorer, and Pb 2+poisonous, in order to improve the stability of PbS, improve the electricity conversion of PbS, researcher has made many explorations, as by polymkeric substance to PbS modifying surface; The surface tissue of PbS nanostructure is improved by controlling pattern; And the compound of two kinds of semi-conductors reaches being separated of photogenerated charge and hole.In numerous inorganic nano materials, research finds, transition metal phosphide, especially nickel phosphide are a kind of high reactivity, high stability and the new catalyst with anti-sulfur poisonous performance.After two kinds of semiconductors coupling, because nickel phosphide has higher conduction level, therefore at flower-shaped PbS/Ni 2in P matrix material, light induced electron is conducive to, to the migration of nickel phosphide conduction band, reducing the compound that photo-generate electron-hole is right, thus reaching effective separation of light induced electron, improve the photoelectric properties of material.In addition, compare with monodimension nanometer material with zero dimension, the nano material of three-dimensional branched structure, not only maintain the quantum effect of nano material, also be provided with the transferring charge continuity of body material, this excellent performance makes the nano material of multidimensional branched structure in catalysis, photoelectric conversion, photoluminescence etc.By Ni 2p is compounded in the surface of three-dimensional flower-shaped PbS material, by regulation and control level structure, electric transmission is limited on particular space, thus plays the effect of insulating electron hole transport passage, reduce charge recombination.The matrix material report be assembled into by PbS at present on other semiconductor materials is more, but the matrix material be compound on PbS by semiconductor material is less, and flower-shaped PbS/Ni 2p matrix material and preparation method thereof has no report.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of flower-shaped PbS/Ni 2the preparation method of P matrix material, raw material is easy to get, and preparation technology is simple, reproducible.
In order to achieve the above object, the technical scheme that the present invention takes is:
A kind of flower-shaped PbS/Ni 2the preparation method of P matrix material, comprises the following steps:
Steps A, adds ethylene glycol (EG) solution of volume 10 ~ 15mL in the first Erlenmeyer flask, and add three acetate hydrate lead and 1 ~ 2mL acetic acid of 1 ~ 2mmol wherein, magnetic agitation, adds 1 ~ 2mmol sublimed sulphur after to be dissolved, ultrasonic disperse is to even; Solution is proceeded in polytetrafluoroethyllining lining, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 120 ~ 160 DEG C of reacting by heating 16 ~ 24h, reaction end naturally cools to room temperature, product is through distilled water, absolute ethanol washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped lead sulfide;
Step B, 12 ~ 18mL distilled water is added in the second Erlenmeyer flask, add the flower-shaped lead sulfide that 0.2 ~ 0.6mmol steps A obtains wherein, magnetic agitation is to dispersed, add 0 ~ 0.3mmol cetyl trimethylammonium bromide (CTAB) and 0 ~ 0.1mmol sodium lauryl sulphate (SDS) mixed surfactant wherein, after being stirred to dissolving, add 0.2 ~ 0.6mmol Nickel dichloride hexahydrate; To be dissolved completely after, solution is proceeded in polytetrafluoroethyllining lining, the yellow phosphorus of 0.2 ~ 0.6mmol is added again in solution, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 160 ~ 200 DEG C of reacting by heating 14 ~ 20h, reaction end naturally cools to room temperature, and product is through distilled water, dehydrated alcohol, benzene washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped PbS/Ni 2p matrix material.
Described polytetrafluoroethyllining lining is 20mL, and compactedness is 60% ~ 80%.
The present invention has following beneficial effect:
The lead sulfide 1, with specific morphology and structure is that nickel phosphide nanoparticle effective compound thereon provides three-dimensional space, solve because nickel phosphide nanoparticle is reunited the technical problem causing catalytic performance lower, effectively prevent the reunion of nickel phosphide nanoparticle, increase the effective contact area with catalytic substrate, improve catalytic performance.
2, flower-shaped PbS/Ni 2in P matrix material, light induced electron is conducive to, to the migration of nickel phosphide conduction band, reducing the compound that photo-generate electron-hole is right, thus reaching effective separation of light induced electron, improve the photoelectric properties of material.
3, cost of the present invention is low, and raw material is easy to get, and preparation technology is simple, reproducible, has potential using value at the fermentation such as photochemical catalysis, photoelectric conversion.
Accompanying drawing explanation
Fig. 1 is the flower-shaped PbS/Ni of the embodiment of the present invention 1 gained 2p matrix material XRD figure.
Fig. 2-a is that flower-shaped lead sulfide SEM prepared by the embodiment of the present invention 1 schemes; Fig. 2-b is PbS/Ni prepared by the embodiment of the present invention 1 2p matrix material SEM schemes.
Fig. 3 is PbS/Ni prepared by the embodiment of the present invention 4 2p matrix material SEM schemes.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
A kind of flower-shaped PbS/Ni 2the preparation method of P matrix material, comprises the following steps:
Steps A, adds ethylene glycol (EG) solution of volume 14mL in the first Erlenmeyer flask, and add three acetate hydrate lead and the 1.2mL acetic acid of 1mmol wherein, magnetic agitation, adds 1.5mmol sublimed sulphur after to be dissolved, ultrasonic disperse is to even; Solution is proceeded in polytetrafluoroethyllining lining, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 140 DEG C of reacting by heating 24h, reaction end naturally cools to room temperature, product is through distilled water, absolute ethanol washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped lead sulfide;
Step B, 16mL distilled water is added in the second Erlenmeyer flask, add the flower-shaped lead sulfide that 0.5mmol steps A obtains wherein, magnetic agitation is to dispersed, add 0.3mmol cetyl trimethylammonium bromide (CTAB) and 0.1mmol sodium lauryl sulphate (SDS) mixed surfactant wherein, after being stirred to dissolving, add 0.25mmol Nickel dichloride hexahydrate; To be dissolved completely after, solution is proceeded in polytetrafluoroethyllining lining, the yellow phosphorus of 0.3mmol is added again in solution, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 180 DEG C of reacting by heating 16h, reaction end naturally cools to room temperature, and product is through distilled water, dehydrated alcohol, benzene washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped PbS/Ni 2p matrix material.
The flower-shaped PbS/Ni that the present embodiment 1 is prepared 2the XRD figure spectrum of P matrix material and SEM picture are as Fig. 1 and Fig. 2-a, Fig. 2-b, and wherein nickel phosphide diameter of nano particles is about 30nm.
Embodiment 2
Change cetyl trimethylammonium bromide (CTAB) consumption in step B in embodiment 1 into 0.0mmol, other conditions are constant, flower-shaped lead sulfide smooth surface in product, and nickel phosphide is not compounded in its surface substantially.
Embodiment 3
Change sodium lauryl sulphate (SDS) consumption in step B in embodiment 1 into 0.0mmol, other conditions are constant, and in product, flower-shaped lead sulfide and nickel phosphide mix, the nickel phosphide nanoparticle that flower-shaped lead sulfide surface recombination is a small amount of.
Embodiment 4
All change cetyl trimethylammonium bromide (CTAB) in step B in embodiment 1 and sodium lauryl sulphate (SDS) consumption into 0.1mmol, other conditions are constant, the nickel phosphide nanoparticle that in product, flower-shaped lead sulfide surface attachment reunion is comparatively serious, and the nickel phosphide nano particle diameter prepared comparatively embodiment 1 large (d ≈ 100nm), as shown in Figure 3.
Embodiment 5
Temperature in step B in embodiment 1 is adjusted to 160 DEG C, and other conditions are constant, and product morphology is similar to embodiment 1, but XRD sign finds that nickel phosphide thing is mutually impure, containing Ni 12p 5assorted peak.
Be described in detail description to specific embodiments of the invention above, and be described the product phenomenon of different embodiments, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.

Claims (3)

1. a flower-shaped PbS/Ni 2the preparation method of P matrix material, is characterized in that, comprises the following steps:
Steps A, adds ethylene glycol (EG) solution of volume 10 ~ 15mL in the first Erlenmeyer flask, and add three acetate hydrate lead and 1 ~ 2mL acetic acid of 1 ~ 2mmol wherein, magnetic agitation, adds 1 ~ 2mmol sublimed sulphur after to be dissolved, ultrasonic disperse is to even; Solution is proceeded in polytetrafluoroethyllining lining, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 120 ~ 160 DEG C of reacting by heating 16 ~ 24h, reaction end naturally cools to room temperature, product is through distilled water, absolute ethanol washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped lead sulfide;
Step B, 12 ~ 18mL distilled water is added in the second Erlenmeyer flask, add the flower-shaped lead sulfide that 0.2 ~ 0.6mmol steps A obtains wherein, magnetic agitation is to dispersed, add 0 ~ 0.3mmol cetyl trimethylammonium bromide (CTAB) and 0 ~ 0.1mmol sodium lauryl sulphate (SDS) mixed surfactant wherein, after being stirred to dissolving, add 0.2 ~ 0.6mmol Nickel dichloride hexahydrate; To be dissolved completely after, solution is proceeded in polytetrafluoroethyllining lining, the yellow phosphorus of 0.2 ~ 0.6mmol is added again in solution, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 160 ~ 200 DEG C of reacting by heating 14 ~ 20h, reaction end naturally cools to room temperature, and product is through distilled water, dehydrated alcohol, benzene washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped PbS/Ni 2p matrix material.
2. the flower-shaped PbS/Ni of one according to claim 1 2the preparation method of P matrix material, is characterized in that: described polytetrafluoroethyllining lining is 20mL, and compactedness is 60% ~ 80%.
3. the flower-shaped PbS/Ni of one according to claim 1 2the preparation method of P matrix material, is characterized in that, comprises the following steps:
Steps A, adds ethylene glycol (EG) solution of volume 14mL in the first Erlenmeyer flask, and add three acetate hydrate lead and the 1.2mL acetic acid of 1mmol wherein, magnetic agitation, adds 1.5mmol sublimed sulphur after to be dissolved, ultrasonic disperse is to even; Solution is proceeded in polytetrafluoroethyllining lining, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 140 DEG C of reacting by heating 24h, reaction end naturally cools to room temperature, product is through distilled water, absolute ethanol washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped lead sulfide;
Step B, 16mL distilled water is added in the second Erlenmeyer flask, add the flower-shaped lead sulfide that 0.5mmol steps A obtains wherein, magnetic agitation is to dispersed, add 0.3mmol cetyl trimethylammonium bromide (CTAB) and 0.1mmol sodium lauryl sulphate (SDS) mixed surfactant wherein, after being stirred to dissolving, add 0.25mmol Nickel dichloride hexahydrate; To be dissolved completely after, solution is proceeded in polytetrafluoroethyllining lining, the yellow phosphorus of 0.3mmol is added again in solution, then polytetrafluoroethyllining lining is sealed in stainless steel mould, in confined conditions by room temperature heating and at 180 DEG C of reacting by heating 16h, reaction end naturally cools to room temperature, and product is through distilled water, dehydrated alcohol, benzene washing, and vacuum 60 DEG C of drying 4 ~ 6h obtain flower-shaped PbS/Ni 2p matrix material.
CN201410816729.6A 2014-12-24 2014-12-24 A kind of flower-shaped PbS/Ni 2the preparation method of P matrix material Expired - Fee Related CN104528812B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105562045A (en) * 2015-12-25 2016-05-11 陕西科技大学 Method for preparing ZnS / Sn4P3 composite

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1958159A (en) * 2006-10-19 2007-05-09 安徽师范大学 Catalyst of phosphatizing nickel, and preparation method
CN101898754A (en) * 2010-08-09 2010-12-01 南开大学 Novel method for preparing nickel phosphide by low-temperature reduction
US20110001092A1 (en) * 2004-05-24 2011-01-06 Drexel University Water soluble nanocrystalline quantum dots
CN102040203A (en) * 2010-11-19 2011-05-04 安徽师范大学 Preparation method and application of nano nickel phosphide

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110001092A1 (en) * 2004-05-24 2011-01-06 Drexel University Water soluble nanocrystalline quantum dots
CN1958159A (en) * 2006-10-19 2007-05-09 安徽师范大学 Catalyst of phosphatizing nickel, and preparation method
CN100430135C (en) * 2006-10-19 2008-11-05 安徽师范大学 Catalyst of phosphatizing nickel, and preparation method
CN101898754A (en) * 2010-08-09 2010-12-01 南开大学 Novel method for preparing nickel phosphide by low-temperature reduction
CN102040203A (en) * 2010-11-19 2011-05-04 安徽师范大学 Preparation method and application of nano nickel phosphide

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105562045A (en) * 2015-12-25 2016-05-11 陕西科技大学 Method for preparing ZnS / Sn4P3 composite

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