CN103848405A - Preparation method of monolayer g-C3N4 nanometer material with monatomic thickness - Google Patents
Preparation method of monolayer g-C3N4 nanometer material with monatomic thickness Download PDFInfo
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- CN103848405A CN103848405A CN201410082698.6A CN201410082698A CN103848405A CN 103848405 A CN103848405 A CN 103848405A CN 201410082698 A CN201410082698 A CN 201410082698A CN 103848405 A CN103848405 A CN 103848405A
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Abstract
The invention discloses a preparation method of a monolayer g-C3N4 nanometer material with monatomic thickness. The preparation method comprises the following steps: step 1, grinding blocky g-C3N4 into powder at room temperature, adding the powder into an acid solution or an alkali solution, uniformly stirring and standing; step 2, uniformly re-stirring the solution obtained in the step 1, performing an ultrasonic treatment, removing a supernatant liquor after precipitating completely, washing with deionized water until the pH is 6-8, drying, grinding, and adding into an organic solvent for the ultrasonic treatment again, and removing the supernatant liquor after precipitating completely; step 3, centrifugally washing the g-C3N4 obtained in the step 2 with absolute ethyl alcohol to obtain the monolayer g-C3N4. The preparation method disclosed by the invention is simple in process, good in repeatability and high in preparation speed. Under the irradiation of a xenon lamp, the photo-catalytic material has high efficiency for producing hydrogen by virtue of decomposition of water and has an obvious effect on degradation of an organic dye. The preparation method disclosed by the invention has the advantages of providing a new idea for preparation and application of a g-C3N4 photo-catalytic material and widening the research range of the photo-catalytic material.
Description
Technical field
The invention belongs to semiconductor nano material technical field, relate to a kind of individual layer g-C
3n
4the preparation method of two dimension photocatalytic nanometer stratified material, especially a kind of individual layer g-C with monatomic thickness
3n
4the preparation method of photocatalyst.
Background technology
G-C
3n
4(Graphene Carbon Nitride, g-C
3n
4) be that a kind of individual layer sheet structure being made up of carbon, nitrogen-atoms is piled up the block g-C forming
3n
4material, because the performances such as its fantabulous electronics, machinery and optics have caused research boom both domestic and external.Especially in photocatalysis field, g-C
3n
4the features such as the electric transmission speed that have the high-specific surface area same with Graphene, is exceedingly fast can improve the catalytic efficiency of photocatalyst material.Due to the g-C of monoatomic layer
3n
4have the specific surface area larger than nitride multilayer carbon, better the ability of photocatalysis efficiency and degradating organic dye has more N atom and C atom in identical area.Therefore, most research team to graphitic carbon nitride, research has great interest.Mainly contain following research: (1) high temperature solid-state method and low-temperature solvent heat method, vapour-phase pyrolysis method and solvent thermal catalysis method have obtained respectively the carbonitride of different-shape, raw material cheapness, and mild condition and method are easy, productive rate is higher, but the method can not be controlled the generation of carbonitride crystal formation.(2) obtained carbon nitride films by electrochemical method.(3) the synthetic carbonitride of high-energy shock wave that utilizes explosive charge to form obtains graphitic carbon nitride, has laminate structure to occur.But these methods all do not obtain individual layer (the about 0.35nm of thickness) atomic arrangement carbonitride truly, are all block g-C which floor or even multilayer are piled up
3n
4.For example, document Jorge A B, Martin D J, Dhanoa M T S, et al.H2and O2Evolution from Water Half-Splitting Reactions by Graphitic Carbon Nitride Materials[J] .The Journal of Physical Chemistry C, 2013,117 (14): in 7178-7185., reported typical stratiform g-C
3n
4, its structure as shown in Figure 1, is cross-linked to form mutually stratiform after a monomer of every three triazine rings composition in this structure, does not form the six-ring single layer structure that six former subrings are closely formed by connecting.
Summary of the invention
For above-mentioned present Research, the object of the invention is to, a kind of individual layer g-C with monatomic thickness is provided
3n
4the preparation method of photocatalyst material, the method preparation condition gentleness, technique is simple, raw material is cheap, reproducible, the material preparing has good photocatalysis performance, and this material is the individual layer g-C with monatomic thickness
3n
4, and there is the six-membered ring structure of graphene-like.
In order to achieve the above object, the present invention adopts following technical solution:
A kind of individual layer g-C with monatomic thickness
3n
4the preparation method of nano material, comprises the steps:
Step 1: under room temperature, by block g-C
3n
4be ground to powdery, join in acid solution or alkaline solution, after stirring, leave standstill;
Step 2: carry out supersound process after step 1 gained solution is stirred again, remove supernatant liquor after precipitation is complete, with deionized water rinsing pH to 6～8; Dry and pulverize lastly, joining and in organic solvent, again carry out supersound process, removing supernatant liquor until precipitation after completely;
Step 3: the g-C that step 2 is obtained
3n
4use dehydrated alcohol centrifuge washing, obtain the g-C of the individual layer with nitrogen-atoms thickness
3n
4.
The present invention also has following other technologies feature:
In described step 1, in described step 1, by block g-C
3n
4after being ground to powdery, cross 140 mesh sieves, join in acid solution or alkaline solution.
In described step 1, g-C
3n
4be less than 0.001 with the mass ratio of acid solution or alkaline solution.
Described acid solution is the H of mass concentration 20%～50%
2sO
4solution.
Described acid solution is the HNO of mass concentration 32%～65%
3solution.
Described acid solution is the HAc solution of mass concentration 50%～99.5%.
Described alkaline solution is KOH or the NaOH solution of volumetric molar concentration 1mol/L～5mol/L.
Described supersound process is carried out in centrifuge tube.
In described supersound process, ultrasonic temperature is 60 DEG C～80 DEG C, and the ultrasonic sound intensity is 40000Hz.
In described supersound process, interval supersound process, accumulative total treatment time 3h.
Compared with prior art, beneficial effect of the present invention:
1, preparation technology is simple, without the heat condition in the time preparing monolayer material, and raw material cheapness, reproducible.
2, the individual layer g with monatomic thickness preparing ?C
3n
4material, and its structure is to have the fine and close six-ring that six former subrings are closely formed by connecting.This structure has larger specific surface area, between atom, ordering is similar to Graphene, has the recombination probability of the reduction photo-generated carrier that Graphene has, can be compound with other semiconductor materials, improve the photocatalysis efficiency of photocatalyst material, widened the research range of photocatalyst material.
Brief description of the drawings
Fig. 1 is document Jorge A B, Martin D J, Dhanoa M T S, et al.H2and O2Evolution from Water Half-Splitting Reactions by Graphitic Carbon Nitride Materials[J] .The Journal of Physical Chemistry C, 2013,117 (14): the typical stratiform g-C reporting in 7178-7185.
3n
4.
Fig. 2 be embodiment 1.1 obtain use 65%HNO
3process g-C
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Fig. 3 be embodiment 1.1 obtain use 65%HNO
3process g-C
3n
4the individual layer g-C obtaining
3n
4the electron-diffraction diagram of photocatalyst material.
Fig. 4 is the individual layer g-C drawing according to Fig. 1 and Fig. 2
3n
4structural representation.
Fig. 5 be embodiment 1.2 obtain use 50%HNO
3process g-C
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Fig. 6 be embodiment 1.3 obtain use 32%HNO
3process g-C
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Fig. 7 is that the Glacial acetic acid of the use 99.5% that obtains of embodiment 2.1 is processed g-C
3n
4the processing g-C obtaining
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Fig. 8 is that the Glacial acetic acid of the use 60% that obtains of embodiment 2.2 is processed g-C
3n
4the processing g-C obtaining
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Fig. 9 is that the Glacial acetic acid of the use 50% that obtains of embodiment 2.3 is processed g-C
3n
4the processing g-C obtaining
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Figure 10 is the KOH solution-treated g-C with 1mol/L that embodiment 3.1 obtains
3n
4the processing g-C obtaining
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Figure 11 is the KOH solution-treated g-C with 3mol/L that embodiment 3.2 obtains
3n
4the processing g-C obtaining
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Figure 12 is the KOH solution-treated g-C with 5mol/L that embodiment 3.3 obtains
3n
4the processing g-C obtaining
3n
4the individual layer g-C obtaining
3n
4the TEM figure of photocatalyst material.
Figure 13 be embodiment 5 obtain use 10%HNO
3process g-C
3n
4the g-C obtaining
3n
4the TEM figure of photocatalyst material.
Figure 14 be embodiment 6 obtain process g-C with deionized water
3n
4the g-C obtaining
3n
4the TEM figure of photocatalyst material.
Figure 15 is the KOH solution-treated g-C with 0.5mol/L that embodiment 7 obtains
3n
4the g-C obtaining
3n
4the TEM figure of photocatalyst material.
Below in conjunction with the drawings and the specific embodiments, the present invention is further explained to explanation.
Embodiment
Embodiment 1.1:
Under room temperature, take 0.0526g g-C
3n
4, in agate mortar, being ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joins 30ml mass concentration and be 65% HNO
3in, after stirring, leave standstill 24h, after again stirring, use intermittent supersound process 3h in the ultrasonic apparatus that centrifuge tube is 40000Hz at 65 DEG C of water-bath medium frequencys, being washed to pH is 6.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 80 DEG C, obtain the g-C of individual layer
3n
4.This individual layer g-C
3n
4the interatomic distance of material is approximately 0.35nm, and six-membered ring structure all can appear in the electron diffraction of any position, and thickness is approximately 0.334nm, and size is greatly between 500nm～1um.As shown in Figure 2 and Figure 3, its single layer structure as shown in Figure 4 for the TEM figure of this material and electron-diffraction diagram.
Embodiment 1.2:
Under room temperature, take 0.0507g g-C
3n
4, in agate mortar, being ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joins 30ml mass concentration and be 50% HNO
3in, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 60 DEG C of water-bath medium frequencys after again stirring, being washed to pH is 6, dries and is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 80 DEG C, obtain the g-C of individual layer
3n
4.This individual layer g-C
3n
4interatomic distance is approximately 0.35nm, and thickness is 0.334nm, and size is approximately 450nm～1um.The TEM of this material schemes as shown in Figure 5.
Embodiment 1.3:
Under room temperature, take 0.0571g g-C
3n
4, in agate mortar, being ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joins 30ml mass concentration and be 32% HNO
3in, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 65 DEG C of water-bath medium frequencys after again stirring, being washed to pH is 6.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 60 DEG C, obtain the g-C of individual layer
3n
4.This individual layer g-C
3n
4interatomic distance is approximately 0.35nm, and six-membered ring structure all can appear in the electron diffraction of any position, and thickness is approximately 0.334nm, and size is greatly between 700nm～5um.The TEM of this material schemes as shown in Figure 6.
Embodiment 2.1:
Under room temperature, take 0.0525g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), join 30ml mass concentration and be in 99.5% HAc, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 80 DEG C of water-bath medium frequencys after again stirring, after being washed to pH and being 6.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 80 DEG C, obtain the g-C of individual layer
3n
4, its thickness is 0.35nm, size is greatly between 5um～20um.The TEM of this monolayer material schemes as shown in Figure 7.
Embodiment 2.2:
Under room temperature, take 0.0546g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), join 30ml mass concentration and be in 60% HAc, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 65 DEG C of water-bath medium frequencys after again stirring, after being washed to pH and being 6.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 70 DEG C, obtain the g-C of individual layer
3n
4, its thickness is 0.35nm, size is greatly between 10um～25um.The TEM of this monolayer material schemes as shown in Figure 8.
Embodiment 2.3:
Under room temperature, take 0.0552g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), join 30ml mass concentration and be in 50% HAc, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 65 DEG C of water-bath medium frequencys after again stirring, after being washed to pH and being 6.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 80 DEG C, obtain the g-C of individual layer
3n
4, its thickness is 0.35nm, size is greatly between 10um～20um.The TEM of this monolayer material schemes as shown in Figure 9.
Embodiment 3.1:
Under room temperature, take 0.0567g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joining 30ml concentration is in the KOH solution of 1mol/L, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 60 DEG C of water-bath medium frequencys after again stirring, being washed to pH is 8.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 80 DEG C, obtain the g-C of individual layer
3n
4, its thickness is 0.35nm, size is greatly between 10um～20um.The TEM of this monolayer material schemes as shown in figure 10.
Embodiment 3.2:
Under room temperature, take 0.0587g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joining 30ml concentration is in the KOH solution of 3mol/L, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 65 DEG C of water-bath medium frequencys after again stirring, being washed to pH is 8.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 80 DEG C, obtain the g-C of individual layer
3n
4, its thickness is 0.35nm, size is greatly between 5um～10um.The TEM of this monolayer material schemes as shown in figure 11.
Embodiment 3.3:
Under room temperature, take 0.0578g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joining 30ml concentration is in the KOH solution of 5mol/L, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 80 DEG C of water-bath medium frequencys after again stirring, being washed to pH is 8.Oven dry is ground to after powder, adds 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 60 DEG C, obtain the g-C of individual layer
3n
4, its thickness is 0.35nm, size is greatly between 10um～25um.The TEM of this monolayer material schemes as shown in figure 12.
Be more than the preferably embodiment that contriver provides, the invention is not restricted to above embodiment.Meanwhile, in process of the test, in contriver, find:
(1) if use acid solution or alkaline solution to g-C
3n
4powder treatment and while not using supersound process, or do not use acid solution or alkaline solution and directly to g-C
3n
4powder adds water while carrying out supersound process, and material color variation is not obvious, and the stratiform g-C obtaining
3n
4material is shown as multilayer and piles up block g-C
3n
4 material.As embodiment 5, embodiment 6.
(2) if when the concentration of the acid solution adding or alkaline solution is lower, g-C
3n
4powdered material color is also substantially unchanged, just deposits to very soon centrifuge tube bottom in supersound process process, and ultrasonic effect is also not obvious, and product colour is darker.As embodiment 5 and embodiment 7.
(3) if when the excessive concentration of the acid solution adding or alkaline solution, for example, in embodiment 4, add the H of excessive concentration
2sO
4stratiform g-C after processing
3n
4material color is too white, stirs rear and H
2sO
4dissolve each other, the centrifugal product that can not get.
Embodiment 4:
Under room temperature, take 0.0587g g-C
3n
4, in agate mortar, being ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joins 30ml concentration and be 98% H
2sO
4in, faint yellow g-C in standing 24h process
3n
4become white floss, the transparence material that becomes colorless after stirring, with H
2sO
4dissolve each other, the centrifugal spawn that can not get.
Embodiment 5:
Under room temperature, take 0.0504g g-C
3n
4, in agate mortar, being ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joins 30ml mass concentration and be 10% HNO
3in, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 65 DEG C of water-bath medium frequencys after again stirring, being washed to pH is 6.At 80 DEG C, dry and grind, the g-C obtaining
3n
4individual layer, its block size and untreated before difference little, there is not considerable change in thickness yet.The TEM of this material schemes as shown in figure 13.
Embodiment 6:
Under room temperature, take 0.0581g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joins in the deionized water of 30ml, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 60 DEG C of water-bath medium frequencys after again stirring.At 80 DEG C, dry and grind, unavailable g-C
3n
4individual layer, its block size and untreated before difference little, there is not considerable change in thickness yet.The TEM of this material schemes as shown in figure 14.
Embodiment 7:
Under room temperature, take 0.0507g g-C
3n
4in agate mortar, be ground to powdery, sieve degranulation footpath is greater than after 0.106mm material (with 140 mesh sieve), joining 30ml concentration is in the KOH solution of 0.5mol/L, after stirring, leave standstill 24h, intermittent supersound process 3h in the ultrasonic apparatus that is 40000Hz at 65 DEG C of water-bath medium frequencys after again stirring, being washed to pH is 8.Add 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry and grind at 80 DEG C, the g-C obtaining
3n
4individual layer, its block size and untreated before difference little, there is not considerable change in thickness yet.The TEM of this material schemes as shown in figure 15.
Claims (10)
1. one kind has the individual layer g-C of monatomic thickness
3n
4the preparation method of nano material, is characterized in that, comprises the steps:
Step 1: under room temperature, by block g-C
3n
4be ground to powdery, join in acid solution or alkaline solution, after stirring, leave standstill;
Step 2: carry out supersound process after step 1 gained solution is stirred again, remove supernatant liquor after precipitation is complete, with deionized water rinsing pH to 6～8; Dry and pulverize lastly, joining and in organic solvent, again carry out supersound process, removing supernatant liquor until precipitation after completely;
Step 3: the g-C that step 2 is obtained
3n
4use dehydrated alcohol centrifuge washing, obtain having the individual layer g-C of nitrogen-atoms thickness
3n
4.
2. the method for claim 1, is characterized in that, in described step 1, in described step 1, by block g-C
3n
4after being ground to powdery, cross 140 mesh sieves, join in acid solution or alkaline solution.
3. the method for claim 1, is characterized in that, in described step 1, and g-C
3n
4be less than 0.001 with the mass ratio of acid solution or alkaline solution.
4. the method for claim 1, is characterized in that, described acid solution is the H of mass concentration 20%～50%
2sO
4solution.
5. the method for claim 1, is characterized in that, described acid solution is the HNO of mass concentration 32%～65%
3solution.
6. method according to claim 1, is characterized in that, described acid solution is the HAc solution of mass concentration 50%～99.5%.
7. method according to claim 1, is characterized in that, described alkaline solution is KOH or the NaOH solution of volumetric molar concentration 1mol/L～5mol/L.
8. the method for claim 1, is characterized in that, described supersound process is carried out in centrifuge tube.
9. the method for claim 1, is characterized in that, in described supersound process, ultrasonic temperature is 60 DEG C～80 DEG C, and the ultrasonic sound intensity is 40000Hz.
10. the method for claim 1, is characterized in that, in described supersound process, and interval supersound process, accumulative total treatment time 3h.
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| CN106542509A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of efficient method for preparing class Graphene carbonitride |
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| CN105692573A (en) * | 2016-03-29 | 2016-06-22 | 中国人民解放军国防科学技术大学 | Preparation method of nano-structure carbon nitride |
| CN106542509A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of efficient method for preparing class Graphene carbonitride |
| CN106542509B (en) * | 2016-10-19 | 2019-01-25 | 张家港市东大工业技术研究院 | A kind of method of efficient preparation class graphene carbonitride |
| CN106752122A (en) * | 2016-11-29 | 2017-05-31 | 东南大学 | One kind nitridation carbon complex, its preparation method and application |
| CN106752122B (en) * | 2016-11-29 | 2019-02-05 | 东南大学 | A kind of nitridation carbon complex, preparation method and application |
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