CN106477539B - A kind of preparation method of ultra-thin graphite phase carbon nitride - Google Patents

A kind of preparation method of ultra-thin graphite phase carbon nitride Download PDF

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CN106477539B
CN106477539B CN201610843167.3A CN201610843167A CN106477539B CN 106477539 B CN106477539 B CN 106477539B CN 201610843167 A CN201610843167 A CN 201610843167A CN 106477539 B CN106477539 B CN 106477539B
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carbon nitride
deionized water
phase carbon
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CN106477539A (en
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沈少华
赵大明
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Xian Jiaotong University
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    • 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
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    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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    • C01P2004/60Particles characterised by their size

Abstract

The present invention provides a kind of preparation methods of ultra-thin graphite phase carbon nitride, first carry out calcination processing to melamine, obtain bulk g-C3N4;Then by blocky g-C3N4It is evenly dispersed in deionized water, ultrasonication processing;The product after ultrasonication is centrifugated again, it is dry to collect solid;Finally by the calcination processing again of the product after drying, i.e. acquisition target product.The present invention realizes the ultra-thin g-C of 0.8~1.2nm (3~4 atomic layers thicks)3N4Be prepared on a large scale to regulate and control with thickness, reaction process organic solvent-free and toxic chemical participate in, and fault of construction and problem of environmental pollution caused by being introduced as impurity can not only be effectively avoided, simultaneously because g-C obtained3N4Nontoxic characteristic can be widely used for photocatalysis, electro-catalysis, bio-sensing, bio-imaging and spintronics.Whole preparation process is easy to operate, and controllability is strong, reproducible, environmentally protective, is suitble to large-scale production.

Description

A kind of preparation method of ultra-thin graphite phase carbon nitride
Technical field
The invention belongs to Material Fields, are related to a kind of ultra-thin (with a thickness of 0.8-12nm) graphite phase carbon nitride (g-C3N4) Preparation method.
Background technique
g-C3N4As a kind of new function nonmetallic materials, there is very high thermal stability and chemical stability, good Thermal conductivity, smaller strip gap value and suitable bandedge placement, specific surface area is controllable, presoma abundance, preparation method letter It is single, environmental-friendly heavy metal free pollution, in addition a variety of excellent characteristics such as its lamellar structure is controllable, so that g-C3N4Photocatalysis, Many new technical fields such as electro-catalysis, bio-sensing, bio-imaging and spintronics have huge potential using value.
Traditional g-C3N4With the biggish multi-slice structure of thickness, and the thickness for reducing stratified material can obtain a system Arrange more excellent physicochemical properties.Due to g-C3N4The van der waals force of interlayer fragility acts on, it is allowed to form thickness Spend lower ultra-thin lamellar structure.Scholar has developed a variety of preparation g-C at present3N4The method of nanometer sheet, such as ultrasonic delamination hair Method, chemical solvent layer stripping, thermal oxide etching method, hydrogen reduction method etc..But in place of the more or less Shortcomings of these methods, than As ultrasonic delamination sends out method, the g-C of acquisition3N4Nanometer sheet thickness is always greater than 2nm (J.Am.Chem.Soc., 2012,135,18); Chemical solvent layer stripping is easy to make g-C3N4Nanometer sheet introduces external source impurity and some harmful functional groups, and it is further to influence it Using (Appl.Catal., B, 2015,163,135);The g-C that directly thermal oxidation etching method obtains3N4The nanometer sheet number of plies is also on the high side, And performance is (Adv.Funct.Mater., 2012,22,4763) to be improved;Hydrogen reducing rule is high under an atmosphere of hydrogen Temperature calcining, there are serious security risk (J.Mater.Chem.A, 2015,3,24237).
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of ultra-thin graphite phase carbon nitride, to solve stone in the prior art Black phase carbon nitride lamellar spacing is big, there are the technologies such as impurity, high, the limitation large-scale serial production of preparation process operation difficulty to ask Topic.
In order to achieve the above objectives, the technical solution adopted by the present invention are as follows:
A kind of preparation method of ultra-thin graphite phase carbon nitride, comprising the following steps:
S1. melamine is placed in crucible, is calcined in ash content furnace, blocky g-C is prepared3N4
S2. by bulk g-C made from step s13N4It is evenly dispersed in deionized water, ultrasonication processing;
S3. product step s2 ultrasonication handled is centrifugated, and is collected solid and is dried in an oven;
S4. the dry solid of step s3 is transferred in crucible, is calcined in ash content furnace, obtain the ultra-thin graphite-phase of target product Carbonitride, the target product with a thickness of 0.8~1.2nm, i.e. 3~4 atomic layer level thickness.
The step s1 specifically: melamine is placed in crucible, is placed into ash content furnace, with 5~10 DEG C/min's Heating rate rises to 500~600 DEG C of calcination temperature from room temperature, then calcines 2~4h at calcination temperatures, then naturally cools to Room temperature obtains blocky g-C3N4
By A g bulk g-C in the step s23N4It is dispersed in B mL deionized water, obtains blocky g-C3N4Deionized water Mixture, A:B=1:(300~500), with ultrasonic cell disruption instrument to blocky g-C3N4Deionized water mixture carries out ultrasound Break process.
In the step s2 when carrying out ultrasonication processing, the probe of ultrasonic cell disruption instrument is protruded into blocky g- C3N4The probe diameter of 1~3cm under deionized water mixture liquid level, ultrasonic cell disruption instrument are 2~20mm, and ultrasonic power is 150~1200W, ultrasonication time are 30~120min.
The revolving speed being centrifugated in the step s3 is 6000~15000r/min, and centrifugation time is 5~15min.
Drying temperature in the step s3 is 60~100 DEG C, and drying time is 6~20h.
The step s4 specifically: the obtained product of step s3 is put into crucible, is placed into ash content furnace, with 5~10 DEG C/heating rate of min rises to 500~600 DEG C of calcination temperature from room temperature, then calcines 2~4h at calcination temperatures, then from It is so cooled to room temperature, obtains target product.
Compared with the existing technology, the invention has the benefit that
Ultra-thin graphite phase carbon nitride (g-C provided by the invention3N4) preparation method, first melamine is carried out at calcining Reason obtains bulk g-C3N4;Then by blocky g-C3N4It is evenly dispersed in deionized water, ultrasonication processing;It is again that ultrasound is broken Product centrifuge separation after broken, it is dry to collect solid;Finally by the product after drying, calcination processing, i.e. acquisition target are produced again Object.The present invention realizes the ultra-thin g-C of 0.8~1.2nm (3~4 atomic layers thicks) using the easily operated method of safety3N4's It is prepared on a large scale, ultra-thin g-C obtained3N4Good dispersion, storage-stable, thickness uniformly, thickness distribution in 1.2nm hereinafter, simultaneously Thickness regulation can be carried out in the range of 0.8~1.2nm.This method organic solvent-free and toxic chemical examination during the reaction Agent participates in, and can not only effectively avoid g-C caused by being introduced as impurity3N4Fault of construction and problem of environmental pollution, simultaneously because being made Ultra-thin g-C3N4Nontoxic characteristic can be widely used in photocatalysis, electro-catalysis, bio-sensing, bio-imaging and spin electricity The fields such as son, are with a wide range of applications.Whole preparation process of the invention is easy to operate, and controllability is strong, reproducible, Raw material is cheap and from a wealth of sources, and heavy metal free pollution, green safe environmental protection improves production efficiency, reduces production cost, fits Close large-scale production.
Further, ultrasonic cell disruption instrument is introduced g-C for the first time by the present invention3N4Material delamination, creative combination make Ultra-thin g-C is prepared with the method for ultrasonic cell-break and thermal polycondensation3N4, make g-C3N4It regroups after lamellar structure is broken, The stacking for inhibiting lamella, has successfully prepared thickness in the ultra-thin g-C of 0.8~1.2nm (3~4 atomic layers thicks) range3N4
Detailed description of the invention
Fig. 1 is ultra-thin g-C made from the embodiment of the present invention 13N4Atomic force microscopy;
Fig. 2 is ultra-thin g-C obtained in the embodiment of the present invention 23N4Atomic force microscopy;
Fig. 3 is ultra-thin g-C obtained in the embodiment of the present invention 33N4Atomic force microscopy;
Fig. 4 is ultra-thin g-C obtained in the embodiment of the present invention 43N4Atomic force microscopy;
Fig. 5 is ultra-thin g-C obtained in the embodiment of the present invention 53N4Atomic force microscopy;
Specific embodiment
As previously mentioned, the present invention is intended to provide a kind of novel environmentally protective thickness is ultra-thin within the scope of 0.8~1.2nm g-C3N4Preparation method, by ultrasonic cell-break method combination thermal polycondensation process prepare, obtain good dispersion, it is storage-stable, The controllable ultra-thin g-C of thickness3N4.Existing methods condition is optimized simultaneously, while guaranteeing final product quality, is selected as far as possible It is preferred that taking the experiment condition that the reaction time is short, raw material usage is few, reaction temperature is low, improves production efficiency, reduces production cost, It overcomes and prepares ultra-thin g-C in the past3N4The problems such as middle thickness is big, low output, is conducive to prepare with scale and practical application.
Generally, technical solution of the present invention includes g-C3N4The broken and g-C of structure3N4Structure regroups.
Specifically, in technical solution of the present invention, g-C3N4The broken of structure can be obtained by ultrasonic cell-break method, Thermal polycondensation process is recycled to make g-C3N4Structure regroups, and obtains the ultra-thin g-C with a thickness of 0.8~1.2nm3N4
Currently preferred specific technical solution specifically includes following reaction step:
S1. melamine is placed in crucible, is placed into ash content furnace, with the heating rate of 5~10 DEG C/min from room temperature 500~600 DEG C of calcination temperature is risen to, then calcines 2~4h at calcination temperatures, then cooled to room temperature, obtains bulk g-C3N4
S2. by A g bulk g-C3N4It is dispersed in B mL deionized water, obtains blocky g-C3N4Deionized water mixture, A: B=1:(300~500), with ultrasonic cell disruption instrument to blocky g-C3N4Deionized water mixture carries out ultrasonication processing; When carrying out ultrasonication processing, the probe of ultrasonic cell disruption instrument is protruded into blocky g-C3N4Deionized water mixture liquid level Lower 1~3cm, the probe diameter of ultrasonic cell disruption instrument are 2~20mm, and ultrasonic power is 150~1200W, when ultrasonication Between be 30~120min;
S3. by step s2 product obtained with speed 5~15min of centrifuging treatment of 6000~15000r/min, Solid is collected in an oven with the dry 6~20h of 60~100 DEG C of temperature;
S4. the obtained product of step s3 is put into crucible, is placed into ash content furnace, with the heating speed of 5~10 DEG C/min Rate rises to 500~600 DEG C of calcination temperature from room temperature, then calcines 2~4h at calcination temperatures, then cooled to room temperature, Obtain the ultra-thin graphite phase carbon nitride of target product, the target product with a thickness of 0.8~1.2nm (3~4 atomic layers thicks).
Technical solution of the present invention is made below in conjunction with attached drawing and several preferred embodiments of the present invention further detailed Explanation.
Embodiment 1
1) melamine is placed in crucible, is placed into ash content furnace, risen to the heating rate of 5 DEG C/min from room temperature 520 DEG C of calcination temperature, then 4h is calcined at calcination temperatures, then cooled to room temperature, obtains blocky g-C3N4
2) bulk g-C made from 500mg step 1) is taken3N4, it is placed in the glassware that volume is 250mL, 200mL is added The probe of ultrasonic cell disruption instrument is inserted into bulk g-C by deionized water3N4In deionized water mixture, probe gos deep into liquid level 1cm, probe diameter 10mm, ultrasonic power 900W, ultrasonication 90min;
3) product of acquisition is centrifugated 15min with the revolving speed of 8000r/min, is then placed in obtained solid after centrifugation Dry 12h in 60 DEG C of vacuum drying oven;
4) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 5 DEG C/min from room temperature liter To 520 DEG C of calcination temperature, then 4h is calcined at calcination temperatures, then with furnace cooled to room temperature, obtain target product.
Embodiment 2
1) melamine is placed in crucible, is placed into ash content furnace, risen to the heating rate of 10 DEG C/min from room temperature 520 DEG C of calcination temperature, then 4h is calcined at calcination temperatures, then cooled to room temperature, obtains blocky g-C3N4
2) bulk g-C made from 500mg step 1) is taken3N4, it is placed in the glassware that volume is 250mL, 150mL is added The probe of ultrasonic cell disruption instrument is inserted into bulk g-C by deionized water3N4In deionized water mixture, probe gos deep into liquid level 1cm, probe diameter 10mm, ultrasonic power 600W, ultrasonication 120min;
3) product of acquisition is centrifugated 5min with the revolving speed of 12000r/min, is then placed in obtained solid after centrifugation Dry 10h in 80 DEG C of vacuum drying oven;
4) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 10 DEG C/min from room temperature 520 DEG C of calcination temperature is risen to, then calcines 4h at calcination temperatures, then with furnace cooled to room temperature, obtains target product.
Embodiment 3
1) melamine is placed in crucible, is placed into ash content furnace, risen to the heating rate of 5 DEG C/min from room temperature 520 DEG C of calcination temperature, then 3h is calcined at calcination temperatures, then cooled to room temperature, obtains blocky g-C3N4
2) bulk g-C made from 500mg step 1) is taken3N4, it is placed in the glassware that volume is 250mL, 200mL is added The probe of ultrasonic cell disruption instrument is inserted into bulk g-C by deionized water3N4In deionized water mixture, probe gos deep into liquid level 1cm, probe diameter 10mm, ultrasonic power 1200W, ultrasonication 60min;
3) product of acquisition is centrifugated 10min with the revolving speed of 10000r/min, then sets obtained solid after centrifugation The dry 12h in 60 DEG C of vacuum drying oven;
4) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 5 DEG C/min from room temperature liter To 520 DEG C of calcination temperature, then 3h is calcined at calcination temperatures, then with furnace cooled to room temperature, obtain target product.
Embodiment 4
1) melamine is placed in crucible, is placed into ash content furnace, risen to the heating rate of 5 DEG C/min from room temperature 550 DEG C of calcination temperature, then 3h is calcined at calcination temperatures, then cooled to room temperature, obtains blocky g-C3N4
2) bulk g-C made from 500mg step 1) is taken3N4, it is placed in the glassware that volume is 250mL, 150mL is added The probe of ultrasonic cell disruption instrument is inserted into bulk g-C by deionized water3N4In deionized water mixture, probe gos deep into liquid level 1cm, probe diameter 10mm, ultrasonic power 900W, ultrasonication 120min;
3) product of acquisition is centrifugated 5min with the revolving speed of 10000r/min, is then placed in obtained solid after centrifugation Dry 12h in 60 DEG C of vacuum drying oven;
4) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 5 DEG C/min from room temperature liter To 550 DEG C of calcination temperature, then 3h is calcined at calcination temperatures, then with furnace cooled to room temperature, obtain target product.
Embodiment 5
1) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 10 DEG C/min from room temperature 580 DEG C of calcination temperature is risen to, then calcines 2h at calcination temperatures, then with furnace cooled to room temperature, obtains target product.
2) bulk g-C made from 500mg step 1) is taken3N4, it is placed in the glassware that volume is 250mL, 200mL is added The probe of ultrasonic cell disruption instrument is inserted into bulk g-C by deionized water3N4In deionized water mixture, probe gos deep into liquid level 1cm, probe diameter 20mm, ultrasonic power 900W, ultrasonication 90min;
3) product of acquisition is centrifugated 15min with the revolving speed of 8000r/min, is then placed in obtained solid after centrifugation Dry 10h in 80 DEG C of vacuum drying oven;
4) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 10 DEG C/min from room temperature 580 DEG C of calcination temperature is risen to, then calcines 2h at calcination temperatures, then with furnace cooled to room temperature, obtains target product.
Embodiment 6
1) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 8 DEG C/min from room temperature liter To 500 DEG C of calcination temperature, then 3.5h is calcined at calcination temperatures, then with furnace cooled to room temperature, obtain target product.
2) bulk g-C made from 500mg step 1) is taken3N4, it is placed in the glassware that volume is 500mL, 250mL is added The probe of ultrasonic cell disruption instrument is inserted into bulk g-C by deionized water3N4In deionized water mixture, probe gos deep into liquid level 2cm, probe diameter 2mm, ultrasonic power 1100W, ultrasonication 30min;
3) product of acquisition is centrifugated 12min with the revolving speed of 6000r/min, is then placed in obtained solid after centrifugation Dry 20h in 70 DEG C of vacuum drying oven;
4) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 8 DEG C/min from room temperature liter To 500 DEG C of calcination temperature, then 3.5h is calcined at calcination temperatures, then with furnace cooled to room temperature, obtain target product.
Embodiment 7
1) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 6 DEG C/min from room temperature liter To 600 DEG C of calcination temperature, then 2.5h is calcined at calcination temperatures, then with furnace cooled to room temperature, obtain target product.
2) bulk g-C made from 500mg step 1) is taken3N4, it is placed in the glassware that volume is 250mL, 180mL is added The probe of ultrasonic cell disruption instrument is inserted into bulk g-C by deionized water3N4In deionized water mixture, probe gos deep into liquid level 3cm, probe diameter 15mm, ultrasonic power 150W, ultrasonication 110min;
3) product of acquisition is centrifugated 8min with the revolving speed of 15000r/min, is then placed in obtained solid after centrifugation Dry 6h in 100 DEG C of vacuum drying oven;
4) solid after drying is transferred in crucible, is placed into ash content furnace, with the heating rate of 6 DEG C/min from room temperature liter To 600 DEG C of calcination temperature, then 2.5h is calcined at calcination temperatures, then with furnace cooled to room temperature, obtain target product.
Fig. 1-Fig. 5 is respectively ultra-thin g-C obtained in 1- of embodiment of the present invention embodiment 53N4Atomic force microscope shine Piece;It can be seen that ultra-thin g-C produced by the present invention from Fig. 1-Fig. 53N4Apparent characteristic uniform, good dispersion with thickness.
It should be pointed out that described above and preferred embodiment may not be interpreted as limiting design philosophy of the invention.Ability Technical thought of the invention can be improved in the form of various and be changed by field technique personnel, and such improvement and change should be understood that In belonging to the scope of protection of the present invention.

Claims (7)

1. a kind of preparation method of ultra-thin graphite phase carbon nitride, which comprises the following steps:
S1. melamine is placed in crucible, is calcined in ash content furnace, blocky g-C is prepared3N4
S2. by bulk g-C made from step s13N4It is evenly dispersed in deionized water, ultrasonication processing;
S3. product step s2 ultrasonication handled is centrifugated, and is collected solid and is dried in an oven;
S4. the dry solid of step s3 is transferred in crucible, is calcined in ash content furnace, obtain the ultra-thin graphite-phase nitridation of target product Carbon, the target product with a thickness of 0.8~1.2nm, i.e. 3~4 atomic layer level thickness.
2. the preparation method of ultra-thin graphite phase carbon nitride according to claim 1, which is characterized in that the step s1 is specific Are as follows: melamine is placed in crucible, is placed into ash content furnace, 500 are risen to from room temperature with the heating rate of 5~10 DEG C/min~ 600 DEG C of calcination temperature, then 2~4h is calcined at calcination temperatures, then cooled to room temperature, obtains blocky g-C3N4
3. the preparation method of ultra-thin graphite phase carbon nitride according to claim 1, it is characterised in that: will in the step s2 Ag bulk g-C3N4It is dispersed in B mL deionized water, obtains blocky g-C3N4Deionized water mixture, A:B=1:(300~ 500), with ultrasonic cell disruption instrument to blocky g-C3N4Deionized water mixture carries out ultrasonication processing.
4. the preparation method of ultra-thin graphite phase carbon nitride according to claim 3, it is characterised in that: in the step s2 When carrying out ultrasonication processing, the probe of ultrasonic cell disruption instrument is protruded into blocky g-C3N41 under deionized water mixture liquid level ~3cm, the probe diameter of ultrasonic cell disruption instrument are 2~20mm, and ultrasonic power is 150~1200W, and the ultrasonication time is 30~120min.
5. the preparation method of ultra-thin graphite phase carbon nitride according to claim 1, it is characterised in that: in the step s3 from The revolving speed of heart separation is 6000~15000r/min, and centrifugation time is 5~15min.
6. the preparation method of ultra-thin graphite phase carbon nitride according to claim 1, it is characterised in that: in the step s3 Drying temperature is 60~100 DEG C, and drying time is 6~20h.
7. the preparation method of ultra-thin graphite phase carbon nitride according to claim 1, which is characterized in that the step s4 is specific Are as follows: the obtained product of step s3 is put into crucible, is placed into ash content furnace, with the heating rate of 5~10 DEG C/min from room temperature 500~600 DEG C of calcination temperature is risen to, then calcines 2~4h at calcination temperatures, then cooled to room temperature, obtains target Product.
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