CN107352519B - A kind of C3N4The preparation method of nano wire - Google Patents

A kind of C3N4The preparation method of nano wire Download PDF

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Publication number
CN107352519B
CN107352519B CN201710645412.4A CN201710645412A CN107352519B CN 107352519 B CN107352519 B CN 107352519B CN 201710645412 A CN201710645412 A CN 201710645412A CN 107352519 B CN107352519 B CN 107352519B
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nano wire
preparation
sodium
salt
oxide
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CN107352519A (en
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张春勇
文颖频
程洁红
赵德建
舒莉
秦恒飞
刘维桥
周月
郑纯智
张国华
周全法
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Jiangsu University of Technology
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Jiangsu University of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0605Binary compounds of nitrogen with carbon
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer

Abstract

The invention discloses a kind of C3N4The preparation method of nano wire by rich nitrogen forerunner and salt or na oxide mixing high-temperature calcination, then is washed, is filtered, drying to get C is arrived3N4Nano wire.Photosensitizer and graphene powder can also be added into water, be protected from light ultrasonic vibration 30min~90min, then 2000 turns~2800 turns 12~20min of centrifugation in washing;System of the present invention is mixed using rich nitrogen forerunner and salt or oxide for the first time, is led to high-temperature calcination, washing method, is prepared C3N4Nano wire, preparation process is simple, and the reaction time is short, environmental friendly, reproducible, easy to industrialized production, prepared C3N4Nano wire has large specific surface area, and photocatalytic activity is up to 86.56%, and C3N4Nano wire pattern, dimensional homogeneity are preferable, reproducible.

Description

A kind of C3N4The preparation method of nano wire
Technical field
The invention belongs to material preparation and photocatalysis technology field, and in particular to be a kind of C3N4The preparation side of nano wire Method.
Background technique
Semiconductor light-catalyst has been a concern in the past few decades.It is obtained because it is widely used in direct hydrolysis Obtain the environmental protection of renewable energy hydrogen and organic polluting water.
In numerous semiconductors, TiO2Since its nontoxic, inexpensive, high stability and excellent photo-catalysis capability become Most study and most promising semiconductor material.But due to big (such as Detitanium-ore-type TiO of its energy gap23.2eV), Can only be using the part ultraviolet light (UV) for accounting for sunlight 3%~4%, and quantum efficiency is low, to limit TiO2Application. Therefore, the methods of doping, metal deposit and preparation of composite material are applied to TiO2Modification, with expectation improve its visible light Photocatalytic activity.
In recent years, a kind of new function material-graphitic carbon nitride (g-C3N4) due to being moved with nonmetal character, high electronics The characteristics of shifting rate, low band gap (2.73eV) and be caused extensive concern.g-C3N4With superior reducing power, photoresponse wave Long reachable 450nm, is expanded to visible-range.But its oxidability ratio TiO2It is weak, in addition, electricity in the photocatalytic process Son-hole further increases separation rate needs.
Summary of the invention
To solve graphitic carbon nitride (g-C of the existing technology3N4) oxidability ratio TiO2It is weak, in photocatalysis The defect that electron-hole pair separation rate in journey needs to further increase, the present invention provide a kind of C3N4The preparation side of nano wire Method.
A kind of C3N4The preparation method of nano wire, by rich nitrogen forerunner and salt or na oxide mixing high-temperature calcination, then wash, Filtering is dried to get C is arrived3N4Nano wire.
Preferably, the rich nitrogen forerunner is any one or more of cyanamide, dicyandiamide and melamine etc..
Further, when washing, photosensitizer and graphene powder are added into water, be protected from light ultrasonic vibration 30min~ 90min, then 2000 turns~2800 turns 12~20min of centrifugation.Preferred photosensitizer is indocyanine green, chlorin e 6 or is two Benzophenone.
Further, the salt be sodium hydroxide, potassium hydroxide, sodium carbonate and sodium bicarbonate etc. any one or it is more Kind.
Further, the na oxide is sodium oxide molybdena or/and sodium peroxide etc..
Further, the mass ratio of rich nitrogen forerunner and salt or na oxide is 0.01~10:0.01~10.
Further, it is 0.01~20 DEG C/min that the condition of high-temperature calcination, which is heating rate, and calcination temperature is 400~550 DEG C, calcination time is 0.5~4h.
The utility model has the advantages that the present invention is mixed using rich nitrogen forerunner and salt or oxide for the first time, lead to high-temperature calcination, washing method, system Standby C out3N4Nano wire, preparation process is simple, and the reaction time is short, environmental friendly, reproducible, easy to industrialized production, prepared C3N4Nano wire has large specific surface area, and photocatalytic activity is up to 86.56%, and C3N4Nano wire pattern, dimensional homogeneity Preferably, reproducible.By the way that photosensitizer is added into water lotion, so that C3N4Nanowire supported a certain amount of photosensitizer, in laser Irradiation under photosensitizer can by oxygen molecule effectively and rapidly be converted into singlet oxygen;The graphene powder in being protected from light ultrasonic vibration But so that C3N4 nano wire is fluffy, spacing is ideal, greatly improves the yield of C3N4 nano wire.
Detailed description of the invention
Fig. 1 is the C of preparation3N4The SEM spectrum of nano wire.
Fig. 2 is the C of preparation3N4The XRD diffracting spectrum of nano wire.
Specific embodiment
Embodiment 1
By 5g melamine forerunner and 1g sodium hydroxide ground and mixed in crucible, it is placed in Muffle furnace with 5 DEG C/min liter Temperature to 500 DEG C of calcining 2h, it is cold go after the deionized water of 10mL is added, refilter, wash, drying to get to C3N4Nano wire.
In order to examine C manufactured in the present embodiment3N4The photocatalysis performance of nano wire carries out photocatalytic degradation methylene to it Blue test: light-catalyzed reaction carries out in cylindrical glass reactor, and using 300W xenon lamp as light source, light source is away from liquid level 20cm;Add magnetic agitation below reaction vessel, be sufficiently mixed solution, keeps concentration and temperature uniformity, catalyst C3N4 Nano wire dosage is 1g/L, methylene blue initial concentration is 20mg/L, and through detecting after 1h, the photocatalytic activity of methylene blue reaches To 84.56%.
Embodiment 2
By 5g melamine forerunner and 5g potassium hydroxide ground and mixed in crucible, it is placed in Muffle furnace with 10 DEG C/min liter Temperature to 520 DEG C of calcining 2.5h, it is cold go after the deionized water of 10mL is added, refilter, wash, drying to get to C3N4Nano wire, The photocatalytic activity of methylene blue reaches 85.67%.
Embodiment 3
5g melamine forerunner and 2g sodium oxide molybdena are mixed in crucible, is placed in Muffle furnace and is warming up to 500 with 4 DEG C/min DEG C calcining 2.5h, it is cold go after the deionized water of 10mL is added, refilter, wash, drying to get to C3N4Nano wire, methylene blue Photocatalytic activity reach 86.56%.
Embodiment 4
5g melamine forerunner and 1.5g sodium carbonate are mixed in crucible, is placed in Muffle furnace and is warming up to 8 DEG C/min 510 DEG C of calcining 2h, it is cold go after the deionized water of 10mL is added, refilter and photosensitizer be added into water and graphene powder carries out water It washes, is protected from light ultrasonic vibration 30min, then 2000 turns of centrifugation 20min dry to get C is arrived3N4Receive nano wire, the light of methylene blue is urged Change degradation rate and reaches 83.21%.
Embodiment 5
1g cyanamide forerunner and 10g sodium peroxide are mixed in crucible, are placed in Muffle furnace with 0.01 DEG C/min heating To 400 DEG C of calcining 4h, it is cold go after the deionized water of 10mL is added, refilter, photosensitizer 0.1mg and Graphene powder be added into water 3mg is washed at end, and ultrasonic vibration 90min is protected from light, and then 2800 turns of centrifugation 12min dry to get C is arrived3N4Receive nano wire, it is sub- The photocatalytic activity of methyl blue reaches 81.29%.
Embodiment 6
2g dicyandiamide forerunner and 9g sodium oxide molybdena are mixed in crucible, is placed in Muffle furnace and is warming up to 550 with 20 DEG C/min DEG C calcining 0.5h, it is cold go after the deionized water of 10mL is added, refilter, photosensitizer 0.05mg and graphene powder be added into water 5mg is washed, and ultrasonic vibration 60min is protected from light, and then 2400 turns of centrifugation 16min dry to get C is arrived3N4Nano wire, methylene Blue photocatalytic activity reaches 84.93%.

Claims (6)

1. a kind of C3N4The preparation method of nano wire, which is characterized in that forge rich nitrogen forerunner and salt or na oxide mixing high temperature It burns, then washes, filters, drying to get C is arrived3N4Nano wire;
When washing, photosensitizer and graphene powder are added into water, is protected from light ultrasonic vibration 30min~90min, then 2000 turns~ 2800 turns of 12~20min of centrifugation.
2. C according to claim 13N4The preparation method of nano wire, it is characterised in that: the rich nitrogen forerunner is single cyanogen Amine, dicyandiamide and melamine any one or more.
3. C according to claim 13N4The preparation method of nano wire, it is characterised in that: the photosensitizer is indoles cyanines Green, chlorin e 6 is benzophenone.
4. C according to claim 13N4The preparation method of nano wire, it is characterised in that: the salt is sodium hydroxide, hydrogen Potassium oxide, sodium carbonate and sodium bicarbonate any one or more;The na oxide is sodium oxide molybdena or/and sodium peroxide.
5. C according to claim 13N4The preparation method of nano wire, it is characterised in that: rich nitrogen forerunner and salt or sodium aoxidize The mass ratio of object is 0.01~10:0.01~10.
6. C according to claim 1 or 53N4The preparation method of nano wire, it is characterised in that: the condition of high-temperature calcination is to rise Warm rate is 0.01~20 DEG C/min, and calcination temperature is 400~550 DEG C, and calcination time is 0.5~4h.
CN201710645412.4A 2017-08-01 2017-08-01 A kind of C3N4The preparation method of nano wire Active CN107352519B (en)

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CN109557142B (en) * 2018-12-27 2021-07-09 东南大学 Quick-response resistance type humidity sensor and preparation method and application thereof
CN109999874A (en) * 2019-03-11 2019-07-12 江苏大学 A kind of richness nitrogen azotized carbon nano pipe photochemical catalyst and preparation method and application
CN113418900A (en) * 2021-07-16 2021-09-21 电子科技大学 Synthesis method of molecular probe with ultrahigh specific surface area and ultrahigh fluorescence intensity
CN113842458A (en) * 2021-10-14 2021-12-28 南京师范大学 Based on C3N4Composite material and preparation method and application thereof

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Application publication date: 20171117

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Contract record no.: X2023980054656

Denomination of invention: A method for preparing C3N4nanowires

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Record date: 20240103