CN106477539A - 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 PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
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Abstract
The invention provides a kind of preparation method of ultra-thin graphite phase carbon nitride, first tripolycyanamide is carried out with calcination processing, obtain block g C3N4；Then by block g C3N4Dispersed in deionized water, ultrasonication process；Again by the product centrifugation after ultrasonication, collect solid and be dried；Finally by dried product calcination processing again, that is, obtain target product.Present invention achieves the ultra-thin g C of 0.8～1.2nm (3～4 atomic layers thick)3N4Be prepared on a large scale and thickness regulation and control, course of reaction organic solvent-free and toxic chemical participate in, and can not only be prevented effectively from and introduce the fault of construction causing and problem of environmental pollution by impurity, simultaneously because the g C being obtained3N4Nontoxic characteristic, can be widely used for photocatalysis, electro-catalysis, bio-sensing, bio-imaging and spintronics.Whole preparation process is simple to operate, and controllability is strong, reproducible, environmental protection, suitable large-scale production.
Description
Technical field
The invention belongs to Material Field, it is related to a kind of ultra-thin (thickness is 0.8-12nm) graphite phase carbon nitride (g-C3N4)
Preparation method.
Background technology
g-C3N4As a kind of new function nonmetallic materials, there is very high heat stability and chemical stability, good
Heat-conductivity conducting, smaller strip gap value and suitable bandedge placement, specific surface area is controlled, presoma abundance, preparation method letter
Single, environmental friendliness heavy metal free pollutes, and adds multiple excellent characteristics such as its lamellar structure is controlled so that g-C3N4Photocatalysis,
Many new technical field such as electro-catalysis, bio-sensing, bio-imaging and spintronics have huge potential using value.
Traditional g-C3N4There are the larger multi-disc Rotating fields of thickness, and the thickness reducing stratified material can obtain one is
Arrange more excellent physicochemical properties.Due to g-C3N4The fragile van der waals force of interlayer acts on so that it can form thickness
Spend lower ultra-thin lamellar structure.Scholar has worked out multiple preparation g-C at present3N4The method of nanometer sheet, such as ultrasonic delamination is sent out
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 easily makes g-C3N4Nanometer sheet introduces external source impurity and some harmful functional groups, affects it further
Application (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 has much room for improvement (Adv.Funct.Mater., 2012,22,4763)；Hydrogen reducing rule is high under an atmosphere of hydrogen
, there is serious potential safety hazard (J.Mater.Chem.A, 2015,3,24237) in temperature calcining.
Content of the invention
It is an object of the invention to provide a kind of preparation method of ultra-thin graphite phase carbon nitride, to solve stone in prior art
Black phase carbon nitride lamellar spacing is big, there is impurity, preparation process operation easier is high, limit the technology such as large-scale mass production asks
Topic.
For reaching above-mentioned purpose, the technical solution used in the present invention is：
A kind of preparation method of ultra-thin graphite phase carbon nitride, comprises the following steps：
S1. tripolycyanamide is placed in crucible, calcines in ash stove, prepare block g-C3N4；
S2. block g-C step s1 being obtained3N4Dispersed in deionized water, ultrasonication process；
S3. the ultrasonication of step s2 is processed the product centrifugation obtaining, collect solid and dry in an oven；
S4. solid step s3 being dried proceeds in crucible, calcines in ash stove, obtains the ultra-thin graphite-phase of target product
Carbonitride, the thickness of described target product is 0.8～1.2nm, i.e. 3～4 atomic layer level thickness.
Described step s1 is specially：Tripolycyanamide is placed in crucible, places in ash stove, with 5～10 DEG C/min's
Heating rate rises to 500～600 DEG C of calcining heat from room temperature, then calcines 2～4h at calcination temperatures, then naturally cools to
Room temperature, obtains block g-C3N4.
By A g bulk g-C in described step s23N4It is dispersed in B mL deionized water, obtain block g-C3N4Deionized water
Mixture, A:B=1:(300～500), with ultrasonic cell disruption instrument to block g-C3N4Deionized water mixture carries out ultrasonic
Break process.
In described step s2 when carrying out ultrasonication process, the probe of ultrasonic cell disruption instrument is stretched into block g-
C3N41～3cm under deionized water mixture liquid level, the probe diameter of ultrasonic cell disruption instrument is 2～20mm, and ultrasonic power is
150～1200W, the ultrasonication time is 30～120min.
In described step s3, the rotating speed of centrifugation is 6000～15000r/min, and centrifugation time is 5～15min.
Drying temperature in described step s3 is 60～100 DEG C, and drying time is 6～20h.
Described step s4 is specially：The product that step s3 is obtained is put in crucible, places in ash stove, with 5～10
DEG C/heating rate of min rises to 500～600 DEG C of calcining heat, then calcines 2～4h at calcination temperatures from room temperature, then from
So it is cooled to room temperature, obtain target product.
With respect to prior art, beneficial effects of the present invention are：
Ultra-thin graphite phase carbon nitride (the g-C that the present invention provides3N4) preparation method, first tripolycyanamide is carried out at calcining
Reason, obtains block g-C3N4；Then by block g-C3N4Dispersed in deionized water, ultrasonication process；Again will be ultrasonic broken
Product centrifugation after broken, collects solid and is dried；Finally by dried product calcination processing again, that is, obtain target and produce
Thing.The present invention achieves the ultra-thin g-C of 0.8～1.2nm (3～4 atomic layers thick) using the easily operated method of safety3N4's
It is prepared on a large scale, prepared ultra-thin g-C3N4Good dispersion, storage-stable, thickness uniformly, thickness distribution in below 1.2nm, and
Thickness regulation and control can be carried out in the range of 0.8～1.2nm.The method organic solvent-free and toxic chemical examination during the course of the reaction
Agent participates in, and can not only be prevented effectively from and introduce, by impurity, the g-C causing3N4Fault of construction and problem of environmental pollution, simultaneously because be obtained
Ultra-thin g-C3N4Nontoxic characteristic is so as to can be widely applied for photocatalysis, electro-catalysis, bio-sensing, bio-imaging and spin electricity
The fields such as son, are with a wide range of applications.The whole preparation process of the present invention is simple to operate, and controllability is strong, reproducible,
Raw material is cheap and wide material sources, and heavy metal free pollutes, and green safety environmental protection improves production efficiency, reduces production cost, fits
Close large-scale production.
Further, ultrasonic cell disruption instrument is introduced g-C by the present invention first3N4Material delamination, creative combination makes
Prepare ultra-thin g-C with the method for ultrasonic cell-break and thermal polycondensation3N4, make g-C3N4Lamellar structure regroups after crushing,
The stacking of suppression lamella, has successfully prepared the ultra-thin g-C in 0.8～1.2nm (3～4 atomic layers thick) scope for the thickness3N4.
Brief description
Fig. 1 is the ultra-thin g-C that the embodiment of the present invention 1 is obtained3N4Atomic force microscopy；
Fig. 2 is the ultra-thin g-C being obtained in the embodiment of the present invention 23N4Atomic force microscopy；
Fig. 3 is the ultra-thin g-C being obtained in the embodiment of the present invention 33N4Atomic force microscopy；
Fig. 4 is the ultra-thin g-C being obtained in the embodiment of the present invention 43N4Atomic force microscopy；
Fig. 5 is the ultra-thin g-C being obtained in the embodiment of the present invention 53N4Atomic force microscopy；
Specific embodiment
As it was previously stated, the present invention is intended to provide a kind of new environmental protection thickness is ultra-thin in the range of 0.8～1.2nm
g-C3N4Preparation method, by ultrasonic cell-break method combine thermal polycondensation process prepare, obtain good dispersion, storage-stable,
The controlled ultra-thin g-C of thickness3N4.Existing methods condition is optimized simultaneously, while ensureing end product quality, selects as far as possible
Preferably take the experiment condition that the response time is short, raw material usage is few, reaction temperature is low, improve production efficiency, reduce production cost,
Overcome and prepared ultra-thin g-C in the past3N4Middle thickness is big, the problems such as yield poorly, beneficial to prepare with scale and practical application.
Generally, technical scheme includes g-C3N4The broken and g-C of structure3N4The regrouping of structure.
Specifically, in technical scheme, 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 that thickness is 0.8～1.2nm3N4.
Currently preferred concrete technical scheme, specifically includes following reactions steps：
S1. tripolycyanamide is placed in crucible, places in ash stove, with the heating rate of 5～10 DEG C/min from room temperature
Rise to 500～600 DEG C of calcining heat, then calcine 2～4h at calcination temperatures, then naturally cool to room temperature, obtain bulk
g-C3N4；
S2. by A g bulk g-C3N4It is dispersed in B mL deionized water, obtain block g-C3N4Deionized water mixture, A:
B=1:(300～500), with ultrasonic cell disruption instrument to block g-C3N4Deionized water mixture carries out ultrasonication process；
When carrying out ultrasonication process, the probe of ultrasonic cell disruption instrument is stretched into block g-C3N4Deionized water mixture liquid level
Lower 1～3cm, the probe diameter of ultrasonic cell disruption instrument is 2～20mm, and ultrasonic power is 150～1200W, during ultrasonication
Between be 30～120min；
S3. product step s2 being obtained with the centrifugation separating treatment 5～15min of 6000～15000r/min,
Collect solid and in an oven 6～20h is dried with 60～100 DEG C of temperature；
S4. the product that step s3 obtains is put in crucible, place in ash stove, with the intensification speed of 5～10 DEG C/min
Rate rises to 500～600 DEG C of calcining heat from room temperature, then calcines 2～4h at calcination temperatures, then naturally cools to room temperature,
Obtain the ultra-thin graphite phase carbon nitride of target product, the thickness of described target product is 0.8～1.2nm (3～4 atomic layers thick).
Below in conjunction with accompanying drawing and some preferred embodiments of the present invention, technical scheme is made further detailed
Explanation.
Embodiment 1
1) tripolycyanamide is placed in crucible, places in ash stove, risen to from room temperature with the heating rate of 5 DEG C/min
520 DEG C of calcining heat, then calcine 4h at calcination temperatures, then naturally cool to room temperature, obtain block g-C3N4；
2) take 500mg step 1) be obtained block g-C3N4, it is placed in the glass drying oven that volume is 250mL, add 200mL
Deionized water, by the block g-C of probe insertion of ultrasonic cell disruption instrument3N4In deionized water mixture, probe gos deep into liquid level
1cm, probe diameter is 10mm, and ultrasonic power is 900W, ultrasonication 90min；
3) by the product obtaining with the rotating speed centrifugation 15min of 8000r/min, then gained solid after centrifugation is placed in
12h is dried in 60 DEG C of vacuum drying oven；
4) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 5 DEG C/min from room temperature liter
To 520 DEG C of calcining heat, then calcine 4h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
Embodiment 2
1) tripolycyanamide is placed in crucible, places in ash stove, risen to from room temperature with the heating rate of 10 DEG C/min
520 DEG C of calcining heat, then calcine 4h at calcination temperatures, then naturally cool to room temperature, obtain block g-C3N4；
2) take 500mg step 1) be obtained block g-C3N4, it is placed in the glass drying oven that volume is 250mL, add 150mL
Deionized water, by the block g-C of probe insertion of ultrasonic cell disruption instrument3N4In deionized water mixture, probe gos deep into liquid level
1cm, probe diameter is 10mm, and ultrasonic power is 600W, ultrasonication 120min；
3) by the product obtaining with the rotating speed centrifugation 5min of 12000r/min, then gained solid after centrifugation is placed in
10h is dried in 80 DEG C of vacuum drying oven；
4) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 10 DEG C/min from room temperature
Rise to 520 DEG C of calcining heat, then calcine 4h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
Embodiment 3
1) tripolycyanamide is placed in crucible, places in ash stove, risen to from room temperature with the heating rate of 5 DEG C/min
520 DEG C of calcining heat, then calcine 3h at calcination temperatures, then naturally cool to room temperature, obtain block g-C3N4；
2) take 500mg step 1) be obtained block g-C3N4, it is placed in the glass drying oven that volume is 250mL, add 200mL
Deionized water, by the block g-C of probe insertion of ultrasonic cell disruption instrument3N4In deionized water mixture, probe gos deep into liquid level
1cm, probe diameter is 10mm, and ultrasonic power is 1200W, ultrasonication 60min；
3) by the product obtaining with the rotating speed centrifugation 10min of 10000r/min, then gained solid after centrifugation is put
12h is dried in 60 DEG C of vacuum drying oven；
4) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 5 DEG C/min from room temperature liter
To 520 DEG C of calcining heat, then calcine 3h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
Embodiment 4
1) tripolycyanamide is placed in crucible, places in ash stove, risen to from room temperature with the heating rate of 5 DEG C/min
550 DEG C of calcining heat, then calcine 3h at calcination temperatures, then naturally cool to room temperature, obtain block g-C3N4；
2) take 500mg step 1) be obtained block g-C3N4, it is placed in the glass drying oven that volume is 250mL, add 150mL
Deionized water, by the block g-C of probe insertion of ultrasonic cell disruption instrument3N4In deionized water mixture, probe gos deep into liquid level
1cm, probe diameter is 10mm, and ultrasonic power is 900W, ultrasonication 120min；
3) by the product obtaining with the rotating speed centrifugation 5min of 10000r/min, then gained solid after centrifugation is placed in
12h is dried in 60 DEG C of vacuum drying oven；
4) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 5 DEG C/min from room temperature liter
To 550 DEG C of calcining heat, then calcine 3h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
Embodiment 5
1) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 10 DEG C/min from room temperature
Rise to 580 DEG C of calcining heat, then calcine 2h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
2) take 500mg step 1) be obtained block g-C3N4, it is placed in the glass drying oven that volume is 250mL, add 200mL
Deionized water, by the block g-C of probe insertion of ultrasonic cell disruption instrument3N4In deionized water mixture, probe gos deep into liquid level
1cm, probe diameter is 20mm, and ultrasonic power is 900W, ultrasonication 90min；
3) by the product obtaining with the rotating speed centrifugation 15min of 8000r/min, then gained solid after centrifugation is placed in
10h is dried in 80 DEG C of vacuum drying oven；
4) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 10 DEG C/min from room temperature
Rise to 580 DEG C of calcining heat, then calcine 2h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
Embodiment 6
1) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 8 DEG C/min from room temperature liter
To 500 DEG C of calcining heat, then calcine 3.5h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
2) take 500mg step 1) be obtained block g-C3N4, it is placed in the glass drying oven that volume is 500mL, add 250mL
Deionized water, by the block g-C of probe insertion of ultrasonic cell disruption instrument3N4In deionized water mixture, probe gos deep into liquid level
2cm, probe diameter is 2mm, and ultrasonic power is 1100W, ultrasonication 30min；
3) by the product obtaining with the rotating speed centrifugation 12min of 6000r/min, then gained solid after centrifugation is placed in
20h is dried in 70 DEG C of vacuum drying oven；
4) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 8 DEG C/min from room temperature liter
To 500 DEG C of calcining heat, then calcine 3.5h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
Embodiment 7
1) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 6 DEG C/min from room temperature liter
To 600 DEG C of calcining heat, then calcine 2.5h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
2) take 500mg step 1) be obtained block g-C3N4, it is placed in the glass drying oven that volume is 250mL, add 180mL
Deionized water, by the block g-C of probe insertion of ultrasonic cell disruption instrument3N4In deionized water mixture, probe gos deep into liquid level
3cm, probe diameter is 15mm, and ultrasonic power is 150W, ultrasonication 110min；
3) by the product obtaining with the rotating speed centrifugation 8min of 15000r/min, then gained solid after centrifugation is placed in
6h is dried in 100 DEG C of vacuum drying oven；
4) dried solid is proceeded in crucible, place in ash stove, with the heating rate of 6 DEG C/min from room temperature liter
To 600 DEG C of calcining heat, then calcine 2.5h at calcination temperatures, then naturally cool to room temperature with stove, obtain target product.
Fig. 1-Fig. 5 is respectively the ultra-thin g-C be obtained in embodiment of the present invention 1- embodiment 53N4Atomic force microscope shine
Piece；The ultra-thin g-C that the present invention is obtained can be seen from Fig. 1-Fig. 53N4Significantly have thickness uniformly, the characteristic of good dispersion.
It is pointed out that described above and preferred embodiment may not be interpreted as limiting the design philosophy of the present invention.Ability
Field technique personnel can by the technical thought of the present invention with various form improvement change, such improvement and change it should be understood that
For belonging in protection scope of the present invention.
Claims (7)
1. a kind of preparation method of ultra-thin graphite phase carbon nitride is it is characterised in that comprise the following steps：
S1. tripolycyanamide is placed in crucible, calcines in ash stove, prepare block g-C3N4；
S2. block g-C step s1 being obtained3N4Dispersed in deionized water, ultrasonication process；
S3. the ultrasonication of step s2 is processed the product centrifugation obtaining, collect solid and dry in an oven；
S4. solid step s3 being dried proceeds in crucible, calcines in ash stove, obtains the nitridation of target product ultra-thin graphite-phase
Carbon, the thickness of described target product is 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 is it is characterised in that described step s1 is concrete
For：Tripolycyanamide is placed in crucible, places in ash stove, rise to 500 with the heating rate of 5～10 DEG C/min from room temperature～
600 DEG C of calcining heat, then calcine 2～4h at calcination temperatures, then naturally cool to room temperature, obtain block g-C3N4.
3. ultra-thin graphite phase carbon nitride according to claim 1 preparation method it is characterised in that：Will in described step s2
Ag bulk g-C3N4It is dispersed in B mL deionized water, obtain block g-C3N4Deionized water mixture, A:B=1:(300～
500), with ultrasonic cell disruption instrument to block g-C3N4Deionized water mixture carries out ultrasonication process.
4. ultra-thin graphite phase carbon nitride according to claim 3 preparation method it is characterised in that：In described step s2
When carrying out ultrasonication process, the probe of ultrasonic cell disruption instrument is stretched into block g-C3N41 under deionized water mixture liquid level
～3cm, the probe diameter of ultrasonic cell disruption instrument is 2～20mm, and ultrasonic power is 150～1200W, and the ultrasonication time is
30～120min.
5. ultra-thin graphite phase carbon nitride according to claim 1 preparation method it is characterised in that：In described step s3 from
The detached rotating speed of the heart is 6000～15000r/min, and centrifugation time is 5～15min.
6. ultra-thin graphite phase carbon nitride according to claim 1 preparation method it is characterised in that：In described 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 is it is characterised in that described step s4 is concrete
For：The product that step s3 is obtained is put in crucible, places in ash stove, with the heating rate of 5～10 DEG C/min from room temperature
Rise to 500～600 DEG C of calcining heat, then calcine 2～4h at calcination temperatures, then naturally cool to room temperature, obtain target
Product.
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