CN105126895B - Graphite phase carbon nitride sheet layer material and preparation method thereof - Google Patents
Graphite phase carbon nitride sheet layer material and preparation method thereof Download PDFInfo
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Abstract
A kind of preparation method of graphite phase carbon nitride sheet layer material, it comprises the following steps:One graphite phase carbon nitride powder is provided, and the graphite phase carbon nitride powder is laid in by heat carrier;By above-mentioned being placed in by heat carrier in tube furnace containing graphite phase carbon nitride powder; and tube furnace is warming up to 150 DEG C ~ 600 DEG C under protective gas atmosphere; 1min ~ 20h is then incubated under ammonia atmosphere and negative pressure state, room temperature is finally cooled to and obtains graphite phase carbon nitride sheet layer material.The present invention also provides a kind of graphite phase carbon nitride sheet layer material prepared by the above method.
Description
Technical field
The present invention relates to a kind of graphite phase carbon nitride sheet layer material and preparation method thereof.
Background technology
The most of visible light catalysts being found at present are all transition metal semi-conducting materials, but this based semiconductor material
Material has that cost is high, photocatalysis efficiency is low, the distinct disadvantage such as not environmentally, seriously constrains it as the extensive of visible light catalyst
Using.King's heart morning et al. found organic semiconducting materials-graphite phase carbon nitride (g-C in 20093N4) there is excellent visible ray
The performance of water hydrogen making is catalytically decomposed(Nat. Mater. 2009, 8, 76).The other material has chemical heat endurance
It is good, without metal, the visible light-responded excellent physical chemical characteristic such as good, cause the extensive concern of domestic and international researchers.Stone
Black phase carbon nitride is generally prepared using thermal polymerization method.However, graphite phase carbon nitride prepared by traditional thermal polymerization method is present
Specific surface area is small, and photo-generated carrier is compound serious, the low shortcoming of sun light utilization efficiency, seriously hinders the extensive of the material and pushes away
Wide application(Adv. Mater. 2015, 27, 2150; Angew. Chem. Int. Ed. 2012, 51, 68).
Research is found, with other similar carbon nitride materials(Such as α-C3N4, β-C3N4)Difference, graphite phase carbon nitride (g-
C3N4) lamellar structure can be peeled off under suitable conditions, and there is larger ratio surface in the graphite phase carbon nitride of lamellar structure
Product, visible light catalytic performance can be improved to a certain extent, therefore is widely believed that and can be effectively improved above mentioned problem.Although
In this way, the preparation of graphite phase carbon nitride sheet layer material and in terms of photocatalytic applications still exist some very important problems.Mesh
Before, the preparation method of graphite phase carbon nitride sheet layer material is mainly comprising the direct stripping method of liquid phase, the hot etching method of air atmosphere and straight
Thermal polymerization is connect, but all there are some obvious shortcomings in these three methods.The direct stripping method efficiency of liquid phase first is low, high energy consumption
And low yield, it is unfavorable for industrialized production, and the graphite phase carbon nitride sheet layer material prepared by the direct stripping method of liquid phase is not
Porous structure, specific surface area is relatively low, makes its visible light catalytic performance relatively low(Adv. Mater. 2013, 25, 2452);Air
The graphite phase carbon nitride sheet layer material that atmosphere heat etching is obtained does not include pore structure equally, and energy gap is big, prevents it from having
Effect utilizes visible ray(Adv. Funct. Mater. 2012, 22, 4763);Direct thermal polymerization technological parameter is difficult to control to,
Cost is high, and the ratio surface of the graphite phase carbon nitride sheet layer material prepared by direct thermal polymerization is smaller, pore structure hardly possible control,
Industrial applications are more difficult(J. Mater. Chem. A 2014, 2, 18924).
The content of the invention
In view of the foregoing, it is necessary to provide a kind of with loose structure and the simple graphite phase carbon nitride lamella material of technique
The preparation method of material.
In addition, there is a need to a kind of graphite phase carbon nitride sheet layer material prepared by the above method of offer.
A kind of preparation method of graphite phase carbon nitride sheet layer material, it comprises the following steps:One graphite phase carbon nitride is provided
Powder, and the graphite phase carbon nitride powder is laid in by heat carrier;And by above-mentioned containing graphite phase carbon nitride powder
It is placed in by heat carrier in heating furnace, and heating furnace is warming up to 150 DEG C ~ 600 DEG C under protective gas atmosphere, then in ammonia
1min ~ 20h is incubated under atmosphere and negative pressure state, room temperature is finally cooled to and obtains graphite phase carbon nitride sheet layer material.
A kind of graphite phase carbon nitride sheet layer material, it has loose structure, and the hole in the loose structure includes running through the stone
The through hole of black phase carbon nitride sheet layer material and the non-through hole for not running through the graphite phase carbon nitride sheet layer material.
Graphite phase carbon nitride sheet layer material prepared by preparation method of the present invention, it, which has, runs through the graphite phase carbon nitride lamella
Loose structure so that the specific surface area of the graphite phase carbon nitride sheet layer material is big, makes it have higher visible light catalytic
Energy.Moreover, having for graphite phase carbon nitride sheet layer material should be significantly increased through the loose structure of the graphite phase carbon nitride lamella
Active site is imitated, while also effectively inhibiting graphite phase carbon nitride piece interlayer because of graphite-phase nitrogen caused by Van der Waals force
Change the phenomenon of carbon plate strata collection, ensure that the catalytic activity of graphite phase carbon nitride sheet layer material.In addition, preparation side of the invention
Graphite phase carbon nitride sheet layer material prepared by method, its pore structure and specific surface area are controllable, and the graphite phase carbon nitride sheet layer material
Preparation method is with low cost and environmental protection.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction figure of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.
Fig. 2 is the SEM figures of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.
Fig. 3 is the TEM figures of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.
Fig. 4 is the nitrogen adsorption curve map of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.
Fig. 5 is the diffusing reflection spectrum of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.
Embodiment
Embodiment of the present invention provides a kind of preparation method of graphite phase carbon nitride sheet layer material, and it comprises the following steps:
Step S1 is laid in by heat carrier there is provided a graphite phase carbon nitride powder, and by the graphite phase carbon nitride powder.
Step S2, by above-mentioned being placed in by heat carrier in tube furnace containing graphite phase carbon nitride powder, and in protectiveness gas
Tube furnace is warming up to 150 DEG C ~ 600 DEG C under body atmosphere, 1min ~ 20h is then incubated under ammonia atmosphere and negative pressure state, finally
It is cooled to room temperature and obtains the graphite phase carbon nitride sheet layer material.The graphite phase carbon nitride lamella has loose structure.
Wherein, it is well known that graphite phase carbon nitride powder has multiple carbonitride layers to be combined with each other by Van der Waals force.Ammonia is used
The Van der Waals force being connected between adjacent carbonitride layer is destroyed in being performed etching to graphite phase carbon nitride powder so that graphite-phase nitrogen
Change toner body to be stripped to form graphite phase carbon nitride sheet layer material, and cause the graphite phase carbon nitride lamella to form described porous
Structure.If temperature is too low during insulation, the expansion effect of the graphite phase carbon nitride powder is bad, if temperature is too high during insulation,
The graphite phase carbon nitride sheet layer material of formation will be decomposed, therefore the holding temperature of present embodiment is 150 DEG C ~ 600 DEG C.And protect
The warm time it is too short or it is long all will influence etching effect, therefore present embodiment soaking time be 1min ~ 20h.The graphite
The thickness of phase carbon nitride sheet layer material is 0.5nm ~ 500nm, the planar dimension of the graphite phase carbon nitride sheet layer material for 10nm ~
100μm.The planar dimension refers to the diameter of a circle with the graphite phase carbon nitride sheet layer material area equation.The loose structure mesopore
Aperture be 1nm ~ 1 μm, the distance between two bore edges is 5nm ~ 2 μm.More specifically, the loose structure includes running through the graphite-phase
The through hole of carbonitride sheet layer material and the non-through hole for not running through the graphite phase carbon nitride sheet layer material.The graphite phase carbon nitride
Carbon nitrogen mol ratio is 3 in sheet layer material:5~4:5.
Specifically, in step S1, the graphite phase carbon nitride powder is by one in melamine, dicyandiamide, urea and thiocarbamide
Kind or a variety of after heat treatment formed.The one kind by heat carrier in graphite paper, crucible, porcelain boat, quartz boat and carbon cloth.
In step S2, one or more of the protective gas in argon gas, nitrogen and helium.The negative pressure state refers to
Pressure is less than or equal to -10kPa state, and the negative pressure state is conducive to graphite phase carbon nitride powder to peel off into graphite phase carbon nitride
Sheet layer material.
It is preferred that, tube furnace is warming up to 200 DEG C ~ 400 DEG C under protective gas atmosphere, then in ammonia atmosphere and negative
10min ~ 6h is incubated under pressure condition.
It is appreciated that the tube furnace can be replaced with other heating furnaces.
The present invention is further described below by comparative example and embodiment.
Comparative example 1
Weigh 8g dicyandiamides to be placed in 30mL alumina crucibles, the crucible containing dicyandiamide is put into tube furnace, nitrogen
550 DEG C of roasting 4h are warming up under atmosphere, grinding obtains graphite phase carbon nitride powder body material.
Comparative example 2
Weigh 10g urea to be placed in 30mL alumina crucibles, the crucible containing urea is put into tube furnace, nitrogen atmosphere
Under be warming up to 550 DEG C roasting 4h, grinding obtain body graphite phase carbon nitride powder body material.
Comparative example 3
Weigh 6g melamines to be placed in 30mL alumina crucibles, the crucible containing melamine be put into tube furnace,
550 DEG C of roasting 4h are warming up under nitrogen atmosphere, grinding obtains graphite phase carbon nitride powder body material.
Comparative example 4
Weigh 6g thiocarbamides to be placed in 30mL alumina crucibles, the crucible containing thiocarbamide is put into tube furnace, nitrogen atmosphere
Under be warming up to 550 DEG C roasting 4h, grinding obtain graphite phase carbon nitride powder body material.
Embodiment 1
The graphite phase carbon nitride powder body material for weighing 1g comparative examples 1 is laid on graphite paper, then will contain graphite-phase nitridation
The graphite paper of toner body is positioned in tube furnace, is warming up to 150 DEG C in a nitrogen atmosphere, then is switched to ammonia atmosphere and in pressure
To be incubated 20h under conditions of -10kPa, it is cooled to room temperature and obtains porous graphite phase carbon nitride sheet layer material.
Embodiment 2
The graphite phase carbon nitride powder body material for weighing 1g comparative examples 2 is laid on crucible, then will contain graphite phase carbon nitride
The crucible of powder is positioned in tube furnace, is warming up to 400 DEG C in a nitrogen atmosphere, then be switched to ammonia atmosphere and pressure for-
1h is incubated under conditions of 10kPa, room temperature is cooled to and obtains porous graphite phase carbon nitride sheet layer material.
Embodiment 3
The graphite phase carbon nitride powder body material for weighing 1g comparative examples 3 is laid on carbon paper, then will contain graphite phase carbon nitride
The carbon paper of powder is positioned in tube furnace, is warming up to 510 DEG C in a nitrogen atmosphere, then be switched to ammonia atmosphere and pressure for-
1h is incubated under conditions of 100kPa, room temperature is cooled to and obtains porous graphite phase carbon nitride sheet layer material.
Embodiment 4
The graphite phase carbon nitride powder body material for weighing 1g comparative examples 4 is laid on carbon paper on quartz boat, then will contain graphite
The carbon paper of phase carbon nitride powder is positioned in tube furnace, is warming up to 600 DEG C under an argon atmosphere, then be switched to ammonia atmosphere and
Pressure is cooled to room temperature and obtains porous graphite phase carbon nitride sheet layer material to be incubated 1min under conditions of -10kPa.
Embodiment 5
The graphite phase carbon nitride powder body material for weighing 0.2g comparative examples 1 is laid on carbon paper on porcelain boat, then will contain graphite
The carbon paper of phase carbon nitride powder is positioned in tube furnace, is warming up to 300 DEG C under helium atmosphere, then be switched to ammonia atmosphere and
Pressure is cooled to room temperature and obtains porous graphite phase carbon nitride sheet layer material to be incubated 0.5h under conditions of -50kPa.
Embodiment 6
The graphite phase carbon nitride powder body material for weighing 1g comparative examples 2 is laid on porcelain boat, then will contain graphite phase carbon nitride
The porcelain boat of powder is positioned in tube furnace, is warming up to 400 DEG C in a nitrogen atmosphere, then be switched to ammonia atmosphere and pressure for-
1h is incubated under conditions of 60kPa, room temperature is cooled to and obtains porous graphite phase carbon nitride sheet layer material.
Embodiment 7
The graphite phase carbon nitride powder body material for weighing 0.3g comparative examples 2 is laid on graphite paper, then will contain graphite-phase nitrogen
The graphite paper for changing toner body is positioned in tube furnace, 500 DEG C is warming up in a nitrogen atmosphere, then be switched to ammonia atmosphere and pressing
Power is cooled to room temperature and obtains porous graphite phase carbon nitride sheet layer material to be incubated 1h under conditions of -30kPa.
Embodiment 8
The graphite phase carbon nitride powder body material for weighing 1g comparative examples 3 is laid on graphite paper, then will contain graphite-phase nitridation
The graphite paper of toner body is positioned in tube furnace, is warming up to 380 DEG C under an argon atmosphere, then is switched to ammonia atmosphere and in pressure
To be incubated 3h under conditions of -10kPa, it is cooled to room temperature and obtains porous graphite phase carbon nitride sheet layer material.
Embodiment 9
The graphite phase carbon nitride powder body material for weighing 0.5g comparative examples 4 is laid on graphite paper, then will contain graphite-phase nitrogen
The graphite paper for changing toner body is positioned in tube furnace, 600 DEG C is warming up in a nitrogen atmosphere, then be switched to ammonia atmosphere and pressing
Power is cooled to room temperature and obtains porous graphite phase carbon nitride sheet layer material to be incubated 2min under conditions of -80kPa.
Fig. 1 is the X-ray powder diffraction figure of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.Can by Fig. 1
To find out, graphite phase carbon nitride sheet layer material includes (100) and (002) characteristic diffraction peak.
Fig. 2 is the SEM figures of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.As seen from Figure 2, should
Graphite phase carbon nitride sheet layer material has the loose structure for substantially running through lamella.
Fig. 3 is the TEM figures of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.The stone as seen from Figure 3
Black phase carbon nitride sheet layer material has the loose structure for substantially running through lamella, and average pore size is about 3nm, two pitch of holes 8nm.
Fig. 4 is the nitrogen adsorption curve map of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.The absorption is bent
Line, which has, significantly returns hysteresis characteristic, shows that the graphite phase carbon nitride sheet layer material has obvious loose structure.
Fig. 5 is the diffusing reflection spectrum of graphite phase carbon nitride sheet layer material prepared by the embodiment of the present invention 3.It can be seen by Fig. 5
Go out, the graphite phase carbon nitride sheet layer material has preferable absorbability to visible ray.
The specific surface area and visible light catalytic performance and embodiment of graphite phase carbon nitride powder in above-mentioned comparative example 1-4
Specific surface area, the average thickness of lamella, the mean level of the sea size of lamella and the visible ray of 1-9 graphite phase carbon nitride sheet layer material
Catalytic performance refers to table 1.Wherein, the visible light catalytic performance is to produce the speed of hydrogen to determine by photocatalysis.This reality
Apply in mode, the rate determination method that photocatalysis produces hydrogen is comprised the following steps that:5mg above-mentioned sample is weighed respectively(Compare
Compared with the graphite phase carbon nitride powder and embodiment 1-9 graphite phase carbon nitride sheet layer material in example 1-4)It is put into 10mL seal glass
In vessel, the H that 2mL fluoroforms, 2mL ethanol and 5mL concentration are 30% is added2O2Mixed solution is made, mixes molten toward containing described
Oxygen is passed through in the glassware of liquid makes its pressure for the glassware is placed in 80 DEG C of water-baths after 1MPa, then passes through
300W xenon lamp carries out the light-catalyzed reaction (wavelength X of light to above-mentioned mixed solution>420nm), after reaction terminates, centrifuge,
Using chromatogram ration analysis hydrogen generation rate.
Table 1
From the above-mentioned data of table 1, compared with graphite phase carbon nitride powder prepared by comparative example 1-4, prepared by embodiment 1-4
Graphite phase carbon nitride sheet layer material(The graphite phase carbon nitride powder of comparative example 1-4 preparations is respectively adopted in raw material)With bigger
Specific surface area, makes it have higher visible light catalytic performance.Moreover, the graphite phase carbon nitride lamella prepared with embodiment 1-4
Material is compared, the specific surface area of graphite phase carbon nitride sheet layer material, the average thickness of lamella and lamella prepared by embodiment 5-9
Mean level of the sea size have differences and make it that visible light catalytic performance is different, show the ratio table of graphite phase carbon nitride sheet layer material
The mean level of the sea size of area, the average thickness of lamella and lamella can be by changing the holding temperature of preparation process, being incubated
Time and pressure are adjusted, so as to adjust the visible light catalytic performance of the graphite phase carbon nitride sheet layer material.
A kind of graphite phase carbon nitride sheet layer material prepared by the above method, the graphite phase carbon nitride sheet layer material has many
Pore structure.The thickness of the graphite phase carbon nitride sheet layer material is 0.5nm ~ 500nm, the graphite phase carbon nitride sheet layer material it is flat
Face size is 10nm ~ 100 μm.The aperture of the loose structure mesopore is 1nm ~ 1 μm, and the air line distance between two bore edges is the μ of 5nm ~ 2
m.More specifically, the loose structure is included through the through hole of the graphite phase carbon nitride sheet layer material and through the graphite-phase nitrogen
Change the non-through hole of carbon plate layer material.Carbon nitrogen mol ratio is 3 in the graphite phase carbon nitride sheet layer material:5~4:5.
It is preferred that, the thickness of the graphite phase carbon nitride sheet layer material is 2nm ~ 200nm, the graphite phase carbon nitride sheet layer material
Planar dimension be 5nm ~ 10 μm.The aperture in the hole is that the air line distance between 2nm ~ 200nm, two bore edges is 5nm ~ 200nm.
The specific surface area of the graphite phase carbon nitride sheet layer material is larger.It is furthermore preferred that the thickness of the graphite phase carbon nitride sheet layer material is
2nm ~ 60nm, the planar dimension of the graphite phase carbon nitride sheet layer material is 50nm ~ 10 μm.
Graphite phase carbon nitride sheet layer material prepared by above-mentioned preparation method, it has through the graphite phase carbon nitride lamella
Loose structure so that the specific surface area of the graphite phase carbon nitride sheet layer material is big, makes it have higher visible light catalytic performance.
Moreover, effectively urging for graphite phase carbon nitride sheet layer material should be significantly increased through the loose structure of the graphite phase carbon nitride lamella
Change avtive spot, while also effectively inhibiting graphite phase carbon nitride piece interlayer because of graphite phase carbon nitride caused by Van der Waals force
The phenomenon of lamella aggregation, ensures that the catalytic activity of graphite phase carbon nitride sheet layer material.In addition, prepared by above-mentioned preparation method
Graphite phase carbon nitride sheet layer material, its pore structure and specific surface area are controllable, and the graphite phase carbon nitride sheet layer material preparation side
Method is with low cost and environmental protection.
In addition, for the person of ordinary skill of the art, can make other each with technique according to the invention design
It is kind corresponding change with deformation, and all these changes and deformation should all belong to the protection domain of the claims in the present invention.
Claims (10)
1. a kind of preparation method of graphite phase carbon nitride sheet layer material, it comprises the following steps:
One graphite phase carbon nitride powder is provided, and the graphite phase carbon nitride powder is laid in by heat carrier;And
It will add by above-mentioned being placed in by heat carrier in heating furnace containing graphite phase carbon nitride powder, and under protective gas atmosphere
Hot stove is warming up to 150 DEG C~600 DEG C, and 1min~20h is then incubated under ammonia atmosphere and negative pressure state, room temperature is finally cooled to
Obtain graphite phase carbon nitride sheet layer material.
2. the preparation method of graphite phase carbon nitride sheet layer material as claimed in claim 1, it is characterised in that:The graphite-phase is nitrogenized
Toner body is after heat treatment formed by the one or more in melamine, dicyandiamide, urea and thiocarbamide.
3. the preparation method of graphite phase carbon nitride sheet layer material as claimed in claim 1, it is characterised in that:It should be selected by heat carrier
One kind from graphite paper, crucible, porcelain boat, quartz boat and carbon cloth.
4. the preparation method of graphite phase carbon nitride sheet layer material as claimed in claim 1, it is characterised in that:The protective gas
One or more in argon gas, nitrogen and helium.
5. the preparation method of graphite phase carbon nitride sheet layer material as claimed in claim 1, it is characterised in that:The negative pressure state is
Pressure is less than or equal to -10kPa.
6. the preparation method of graphite phase carbon nitride sheet layer material as claimed in claim 1, it is characterised in that:Heating furnace heating temperature
Degree is to 200 DEG C~400 DEG C, and soaking time is 10min~6h.
7. a kind of graphite phase carbon nitride sheet layer material as prepared by the preparation method of any one of claim 1~6, its feature exists
In:The graphite phase carbon nitride sheet layer material has loose structure, and the hole in the loose structure includes running through the graphite phase carbon nitride
The through hole of sheet layer material and the non-through hole for not running through the graphite phase carbon nitride sheet layer material.
8. graphite phase carbon nitride sheet layer material as claimed in claim 7, it is characterised in that:The graphite phase carbon nitride sheet layer material
Thickness be 0.5nm~500nm, the planar dimension of the graphite phase carbon nitride sheet layer material is 10nm~100 μm.
9. graphite phase carbon nitride sheet layer material as claimed in claim 7, it is characterised in that:The aperture in the hole in the loose structure
For 1nm~1 μm, the air line distance between two bore edges is 5nm~2 μm.
10. graphite phase carbon nitride sheet layer material as claimed in claim 7, it is characterised in that:The graphite phase carbon nitride lamella material
Carbon nitrogen mol ratio is 3 in material:5~4:5.
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CN107311126B (en) * | 2017-08-15 | 2019-07-16 | 哈尔滨工业大学 | A kind of preparation method and applications with accordion graphite phase carbon nitride |
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CN110148713B (en) * | 2018-02-12 | 2021-02-05 | 澳门大学 | Carbon-coated nitrogen-rich g-C3N4And anode material and preparation method thereof |
CN109755640A (en) * | 2019-03-13 | 2019-05-14 | 西安交通大学 | A kind of preparation method of composite solid polymer electrolyte |
CN110148735B (en) * | 2019-06-03 | 2022-03-22 | 河南师范大学 | Preparation method of self-supporting graphite phase carbon nitride/conductive polymer composite sulfur positive electrode material |
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