CN106077688B - A kind of Sn@C@g C3N4Nano-complex and preparation method thereof - Google Patents

A kind of Sn@C@g C3N4Nano-complex and preparation method thereof Download PDF

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CN106077688B
CN106077688B CN201610397220.1A CN201610397220A CN106077688B CN 106077688 B CN106077688 B CN 106077688B CN 201610397220 A CN201610397220 A CN 201610397220A CN 106077688 B CN106077688 B CN 106077688B
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nano
complex
negative electrode
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anode
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CN106077688A (en
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刘先国
赵成云
陈浩
孙玉萍
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Anhui University of Technology AHUT
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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Abstract

The invention discloses a kind of Sn@C@g C3N4Nano-complex and preparation method thereof, belong to technical field of nanometer material preparation.The nano complexes material microstructure is that Sn@C nuclear shell structure nanos capsule is embedded in g C3N4In nanometer sheet, the particle diameter of the Nano capsule is 5~100nm.The present invention uses plasma-arc electric discharge, glass putty and melamine powder are pressed into block as anode target material material by certain atomic percent, using graphite as cathode material, argon gas and methane are quoted as working gas, certain distance is kept between negative electrode graphite electrode and anode target material tin melamine powder block, arc discharge is played between anode and negative electrode, produces Sn C g C3N4Nano-complex.The nano-complex visible light catalysis activity is high and preparation process is simple, without postprocessing working procedures, cost is low, is easily achieved industrialized production.

Description

A kind of Sn@C@g-C3N4Nano-complex and preparation method thereof
Technical field
The invention belongs to technical field of material, and in particular to a kind of Sn@C@g-C3N4Nano-complex and its preparation side Method.
Background technology
Current economic society is fast-developing, and problem of environmental pollution has a strong impact on the survival and development of the mankind.Photocatalysis technology The pollutant in solar energy degraded and mineralising environment can be absorbed, converts solar energy into storable Hydrogen Energy, therefore solving energy There is important application prospect in terms of source and environmental problem.The core of photocatalysis technology is the design and conjunction of high-efficiency photocatalysis material Into.g-C3N4A novel semi-conductor similar to graphite-structure, have suitable semiconductor width (about 2.7eV), Stability Analysis of Structures, Acid and alkali-resistance, the advantages that nontoxic and bio-compatibility is good, cost is low and is easy to chemical modification, have been used for photocatalytic synthesis into anti- Answer, in photocatalysis price reduction pollutant, photodissociation aquatic products hydrogen and production oxygen and redox reaction.g-C3N4Photo-generate electron-hole is to dividing It is low from efficiency, so as to cause photocatalysis performance relatively low.Heterojunction structure is advantageous to the separation in electronics and hole pair, so as to improve quantum Efficiency.Nano metal particles stability is poor, the defects of easily reuniting limits its extensive use, but and g-C3N4After compound, its is preferable Electric conductivity promote electronics transfer, enhance g-C3N4Photocatalytic activity.Such as：Patent 20120387276.0 discloses one kind Au/g-C3N4The preparation method of compound micro Nano material.It is using by g-C3N4Powder is added in chlorauric acid solution and is made Suspension, then heat, add sodium citrate, stir drying, that is, obtain Au/g-C3N4Compound micro Nano material.Patent 201310606627.7 disclose metal/class graphitic nitralloy carbon composite catalyst and preparation method thereof.Its method is by class stone Solution is made in black carbonitride, adds silver nitrate under agitation, opens light source, carries out photo-reduction, obtains final product.Patent 201310220362.7 disclose the preparation method and application for carrying the mesoporous graphite phase carbon nitride visible light catalysts of Co.The material is Cyanamide is first obtained into mesoporous graphite phase carbon nitride, then by the precursor solution immersion of cobalt, and in Muffle by high-temperature roasting Secondary high-temperature roasting is carried out in stove, loaded catalyst Co/g-C is made3N4.Through retrieval, Sn@C@g-C3N4Nano-complex is not Appear in the newspapers.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of Sn@C@g-C3N4Nano-complex and its system Preparation Method.
The invention provides a kind of Sn@C@g-C3N4Nano-complex, the nano-complex microstructure are Sn@C nucleocapsid knots Structure Nano capsule is embedded in g-C3N4In nanometer sheet, the particle diameter of the Nano capsule is 5~100nm.
Present invention also offers above-mentioned Sn@C@g-C3N4The preparation method of nano-complex, the material are to utilize plasma Arc-discharge technique, original position is prepared under working gas；Wherein：
Graphite electrode is used as negative electrode, tin-melamine powder block is anode target material, is protected between negative electrode and anode target material Hold 2~30mm distance；The voltage of arc discharge is 10~40V；Working gas is argon gas and methane gas.
The anode target material is tin-melamine powder block, by glass putty and melamine powder in pressure 1MPa~1Gpa Under be pressed into anode target material material of the block as plasma arc furnace, the quality percentage in the anode target material material shared by tin Than for 70~90%.
The partial pressure of the argon working gas is 0.01~0.5MPa, and the partial pressure of methane gas is 0.01~0.3MPa.
Compared with the prior art, it is of the invention to have the prominent advantages that：
1) present invention has prepared Sn@C@g-C first3N4Nano-complex；
2) preparation process condition of the present invention is simple, easily controllable, disposably generates product, is Sn@C@g-C3N4It is nano combined The practical application of thing provides condition；
3) Sn@C@g-C prepared by the present invention3N4Nano-complex, because Sn@C presence can preferably increase electric conductivity Can, electronics transfer is promoted, makes Sn@C@g-C3N4Nano-complex has good photocatalytic activity, for organic pollution Degraded provides effective solution method.
Brief description of the drawings
Fig. 1 prepares Sn@C@g-C for the present invention3N4The schematic device of nano-complex；
Label in figure：1st, upper lid；2nd, negative electrode；3rd, valve；4th, anode target material；5th, observation window；6th, baffle plate；7th, copper anode；8th, press from both sides Head；9th, graphite crucible；10th, DC pulse power supply；A, cooling water；B, argon gas；C, methane gas.
Fig. 2 is Sn@C@g-C prepared by the embodiment of the present invention 13N4X-ray diffraction (XRD) collection of illustrative plates of nano-complex；
According to JCPDS PDF cards, nano-complex principal phase can be retrieved and formed for Sn crystalline phases.2 θ=27.5 ° and 13 ° Two peaks at place are g-C3N4The characteristic peak of (JCPDS cards, No.87-1562), because C is in shell, so XRD can not be detected C phases.
Fig. 3 is Sn@C@g-C prepared by the embodiment of the present invention 13N4Transmission electron microscope (TEM) figure of nano-complex Picture；
As can be seen from the figure Sn@C nanos capsule is distributed in g-C3N4In nanometer sheet, the particle diameter of its Nano capsule for 5~ 100nm。
Fig. 4 is Sn@C@g-C prepared by the embodiment of the present invention 13N4The high resolution transmission electron microscopy of nano-complex Picture；
As can be seen from the figure gained Sn@C@g-C3N4Nano-complex is that Sn@C nuclear shell structure nanos capsule is embedded in g- C3N4In nanometer sheet.
Fig. 5 is Sn@C@g-C prepared by the embodiment of the present invention 13N4Nano-complex and g-C3N4To the degradability of methyl orange Figure (dosage 0.03g/25ml methyl orange solutions) can be compared；
Gained Sn@C@g-C as we can see from the figure3N4The photocatalysis performance of nano-complex is with respect to g-C3N4Have obvious Improve.
Embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
Lid 1 on device shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, institute's consumable anode target 4 Composition is pure tin powder and melamine powder (mass ratio 90:10) block being pressed into, it is placed on the copper anode 7 of logical cooling water, in copper It is graphite crucible 9 between anode 7 and anode target material 4.30mm distance is kept between negative electrode 2 and anode target material 4.On lid mounted device Lid 1, lead to cooling water a, after whole operating room is vacuumized by valve 3, be passed through argon gas b and methane gas c, the partial pressure of argon gas is 0.5MPa, the partial pressure of methane gas is 0.3MPa, connects DC pulse power supply 10, voltage 40V, work is adjusted during arc discharge Make electric current to keep relative stability with voltage, Sn@C@g-C are made3N4Nano-complex.The nano-complex microstructure is Sn@C Nuclear shell structure nano capsule is embedded in g-C3N4Nanometer sheet, wherein：The particle diameter of Sn@C nano capsules is 5~100nm, such as Fig. 3, Fig. 4 institute Show.Photocatalysis performance of the nano-complex to methyl orange is tested, as shown in figure 5, finding its photocatalysis performance with respect to g-C3N4Have It is obvious to improve.
Embodiment 2
Lid 1 on device shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, institute's consumable anode target 4 Composition is pure tin powder and melamine powder (mass ratio 70:30) block being pressed into, it is placed on the copper anode 7 of logical cooling water, in copper It is graphite crucible 9 between anode 7 and anode target material 4.30mm distance is kept between negative electrode 2 and anode target material 4.On lid mounted device Lid 1, lead to cooling water a, after whole operating room is vacuumized by valve 3, be passed through argon gas b and methane gas c, the partial pressure of argon gas is 0.5MPa, the partial pressure of methane gas is 0.3MPa, connects DC pulse power supply 10, voltage 10V, work is adjusted during arc discharge Make electric current to keep relative stability with voltage, Sn@C@g-C are made3N4Nano-complex.The nano-complex microstructure is Sn@C Nuclear shell structure nano capsule is embedded in g-C3N4Nanometer sheet, wherein：The particle diameter of Sn@C nano capsules is 5~100nm.
Embodiment 3
Lid 1 on device shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, institute's consumable anode target 4 Composition is pure tin powder and melamine powder (mass ratio 90:10) block being pressed into, it is placed on the copper anode 7 of logical cooling water, in copper It is graphite crucible 9 between anode 7 and anode target material 4.30mm distance is kept between negative electrode 2 and anode target material 4.On lid mounted device Lid 1, lead to cooling water a, after whole operating room is vacuumized by valve 3, be passed through argon gas b and methane gas c, the partial pressure of argon gas is 0.5MPa, the partial pressure of methane gas is 0.3MPa, connects DC pulse power supply 10, voltage 20V, work is adjusted during arc discharge Make electric current to keep relative stability with voltage, Sn@C@g-C are made3N4Nano-complex.The nano-complex microstructure is Sn@C Nuclear shell structure nano capsule is embedded in g-C3N4Nanometer sheet, wherein：The particle diameter of Sn@C nano capsules is 5~100nm.
Embodiment 4
Lid 1 on device shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, institute's consumable anode target 4 Composition is pure tin powder and melamine powder (mass ratio 80:20) block being pressed into, it is placed on the copper anode 7 of logical cooling water, in copper It is graphite crucible 9 between anode 7 and anode target material 4.30mm distance is kept between negative electrode 2 and anode target material 4.On lid mounted device Lid 1, lead to cooling water a, after whole operating room is vacuumized by valve 3, be passed through argon gas b and methane gas c, the partial pressure of argon gas is 0.2MPa, the partial pressure of methane gas is 0.2MPa, connects DC pulse power supply 10, voltage 30V, work is adjusted during arc discharge Make electric current to keep relative stability with voltage, Sn@C@g-C are made3N4Nano-complex.The nano-complex microstructure is Sn@C Nuclear shell structure nano capsule is embedded in g-C3N4Nanometer sheet, wherein：The particle diameter of Sn@C nano capsules is 5~100nm.
Embodiment 5
Lid 1 on device shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, institute's consumable anode target 4 Composition is pure tin powder and melamine powder (mass ratio 80:20) block being pressed into, it is placed on the copper anode 7 of logical cooling water, in copper It is graphite crucible 9 between anode 7 and anode target material 4.30mm distance is kept between negative electrode 2 and anode target material 4.On lid mounted device Lid 1, lead to cooling water a, after whole operating room is vacuumized by valve 3, be passed through argon gas b and methane gas c, the partial pressure of argon gas is 0.01MPa, the partial pressure of methane gas is 0.01MPa, connects DC pulse power supply 10, voltage 40V, is adjusted during arc discharge Operating current keeps relative stability with voltage, and Sn@C@g-C are made3N4Nano-complex.The nano-complex microstructure is Sn@ C nuclear shell structure nanos capsule is embedded in g-C3N4Nanometer sheet, wherein：The particle diameter of Sn@C nano capsules is 5~100nm.

Claims (1)

  1. A kind of 1. Sn@C@g-C3N4Nano-complex, it is characterised in that the nano-complex microstructure is Sn@C core shell structures Nano capsule is embedded in g-C3N4In nanometer sheet；The particle diameter of the Nano capsule is 5~100nm；
    The nano-complex is to utilize plasma arc discharge technology, and original position is prepared under working gas；Wherein：
    Graphite electrode is used as negative electrode, tin-melamine powder block is anode target material, and 2 are kept between negative electrode and anode target material ~30mm distance；The voltage of arc discharge is 10~40V；The working gas is argon gas and methane gas；The plate target Mass percent in material shared by tin is 70~90%；The partial pressure of the argon gas is 0.01~0.5MPa, the partial pressure of methane gas For 0.01~0.3MPa.
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CN102623669A (en) * 2012-03-31 2012-08-01 大连理工大学 Preparation method and application of carbon tin nanometer composite powder
CN104415786A (en) * 2013-09-04 2015-03-18 安徽大学 Method for quickly preparing quasi-graphite-structure carbon nitride material by adopting microwave heating
CN103586064A (en) * 2013-11-26 2014-02-19 中国科学院福建物质结构研究所 Metal/graphite-like carbon nitride compound catalyst and preparing method thereof
KR102454572B1 (en) * 2014-06-19 2022-10-13 잉크론 오이 Composition having siloxane polymer and particle
CN105195190A (en) * 2015-07-06 2015-12-30 阜阳师范学院 Heterojunction photocatalyst SnS2/g-C3N4 as well as preparation method and application thereof
CN105428618B (en) * 2015-11-17 2017-12-26 大连理工大学 A kind of preparation method and applications of core-shell type carbon-clad metal sulfide nano-complex particle
CN105562052A (en) * 2016-01-06 2016-05-11 南昌航空大学 Hydrothermal method for preparing g-C3N4/SnS2 composite photocatalyst with multi-layer hierarchical structure

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