CN103848405B - A kind of individual layer g-C with monoatomic thickness 3n 4the preparation method of nano material - Google Patents

A kind of individual layer g-C with monoatomic thickness 3n 4the preparation method of nano material Download PDF

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CN103848405B
CN103848405B CN201410082698.6A CN201410082698A CN103848405B CN 103848405 B CN103848405 B CN 103848405B CN 201410082698 A CN201410082698 A CN 201410082698A CN 103848405 B CN103848405 B CN 103848405B
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individual layer
supersound process
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stirring
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CN103848405A (en
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樊君
马永宁
刘恩周
胡晓云
李兴华
代宏哲
武慧童
樊骁
李银叶
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Northwest University
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Abstract

The invention discloses a kind of individual layer g-C with monoatomic thickness 3n 4the preparation method of photocatalyst material: step 1: under room temperature, by block g-C 3n 4be ground to powdery, join in acid solution or alkaline solution, leave standstill after stirring; Step 2: carry out supersound process after again being stirred by step 1 gained solution, to be precipitated completely after remove supernatant liquor, with deionized water rinsing pH to 6 ~ 8; Dry and grind, joining in organic solvent and again carry out supersound process, to be precipitated completely after remove supernatant liquor; Step 3: the g-C that step 2 is obtained 3n 4use dehydrated alcohol centrifuge washing, namely obtain the g-C of individual layer 3n 4.Preparation technology of the present invention is simple, reproducible, and preparation speed is fast.Under xenon lamp irradiates, this photocatalyst material hydrogen production by water decomposition efficiency is high, degradating organic dye successful.The present invention is g-C 3n 4the preparations and applicatio of photocatalyst material provides new approaches, has widened the research range of photocatalyst material.

Description

A kind of individual layer g-C with monoatomic thickness 3n 4the preparation method of nano material
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 monoatomic thickness 3n 4the preparation method of photocatalyst.
Background technology
G-C 3n 4(GrapheneCarbonNitride, g-C 3n 4) be the block g-C that a kind of individual layer sheet structure be made up of carbon, nitrogen-atoms is piled up 3n 4material, causes research boom both domestic and external due to performances such as its fantabulous electronics, machinery and optics.Especially in photocatalysis field, g-C 3n 4there is the catalytic efficiency that the features such as the high-specific surface area same with Graphene, the electric transmission speed that is exceedingly fast can improve photocatalyst material.Due to the g-C of monoatomic layer 3n 4there is the specific surface area larger than nitride multilayer carbon, the ability of better photocatalysis efficiency and degradating organic dye, in identical area, have more atom N and C atom.Therefore, current most of research team has great interest to graphitic carbon nitride research.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 obtain the carbonitride of different-shape respectively, cheaper starting materials, mild condition and method is easy, productive rate is higher, but the method can not control the generation of carbonitride crystal formation.(2) carbon nitride films is obtained by electrochemical method.(3) the high-energy shock wave synthesis carbonitride utilizing explosive charge to be formed obtains graphitic carbon nitride, namely has laminate structure to occur.But these methods all do not obtain individual layer (thickness is about 0.35nm) atomic arrangement carbonitride truly, are all block g-C which floor or even multilayer are piled up 3n 4.Such as, document JorgeAB, MartinDJ, DhanoaMTS, etal.H2andO2EvolutionfromWaterHalf-SplittingReactionsbyG raphiticCarbonNitrideMaterials [J] .TheJournalofPhysicalChemistryC, 2013, report typical lamellar g-C in 117 (14): 7178-7185. 3n 4, its structure as shown in Figure 1, is cross-linked to form stratiform mutually after every three triazine rings form a monomer in this structure, does not form the six-ring single layer structure of six atom ring compact siro spinning technology.
Summary of the invention
For above-mentioned present Research, the object of the invention is to, a kind of individual layer g-C with monoatomic thickness is provided 3n 4the preparation method of photocatalyst material, the method preparation condition is gentle, technique simple, cheaper starting materials, reproducible, and the material prepared has good photocatalysis performance, and this material is the individual layer g-C with monoatomic 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 monoatomic 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, leave standstill after stirring;
Step 2: carry out supersound process after again being stirred by step 1 gained solution, to be precipitated completely after remove supernatant liquor, with deionized water rinsing pH to 6 ~ 8; Dry and pulverize last, joining in organic solvent and again carry out supersound process, to be precipitated completely after remove supernatant liquor;
Step 3: the g-C that step 2 is obtained 3n 4use dehydrated alcohol centrifuge washing, namely 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 4cross 140 mesh sieves after being ground to powdery, join in acid solution or alkaline solution.
In described step 1, g-C 3n 40.001 is less than 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, cumulative processing time 3h.
Compared with prior art, beneficial effect of the present invention:
1, preparation technology is simple, without the need to the high temperature heating conditions when preparing monolayer material, and cheaper starting materials, reproducible.
2, the individual layer g with monoatomic thickness prepared ?C 3n 4material, and its structure is the fine and close six-ring with six atom ring compact siro spinning technology.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 with other semiconductor material compounds, improve the photocatalysis efficiency of photocatalyst material, widen the research range of photocatalyst material.
Accompanying drawing explanation
Fig. 1 is document JorgeAB, MartinDJ, DhanoaMTS, etal.H2andO2EvolutionfromWaterHalf-SplittingReactionsbyG raphiticCarbonNitrideMaterials [J] .TheJournalofPhysicalChemistryC, 2013, the typical lamellar g-C reported in 117 (14): 7178-7185. 3n 4.
Fig. 2 be embodiment 1.1 obtain use 65%HNO 3process g-C 3n 4the individual layer g-C obtained 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 obtained 3n 4the electron-diffraction diagram of photocatalyst material.
Fig. 4 is the individual layer g-C drawn 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 obtained 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 obtained 3n 4the TEM figure of photocatalyst material.
Fig. 7 is the Glacial acetic acid process g-C of the use 99.5% that embodiment 2.1 obtains 3n 4the process g-C obtained 3n 4the individual layer g-C obtained 3n 4the TEM figure of photocatalyst material.
Fig. 8 is the Glacial acetic acid process g-C of the use 60% that embodiment 2.2 obtains 3n 4the process g-C obtained 3n 4the individual layer g-C obtained 3n 4the TEM figure of photocatalyst material.
Fig. 9 is the Glacial acetic acid process g-C of the use 50% that embodiment 2.3 obtains 3n 4the process g-C obtained 3n 4the individual layer g-C obtained 3n 4the TEM figure of photocatalyst material.
Figure 10 is the KOH solution process g-C with 1mol/L that embodiment 3.1 obtains 3n 4the process g-C obtained 3n 4the individual layer g-C obtained 3n 4the TEM figure of photocatalyst material.
Figure 11 is the KOH solution process g-C with 3mol/L that embodiment 3.2 obtains 3n 4the process g-C obtained 3n 4the individual layer g-C obtained 3n 4the TEM figure of photocatalyst material.
Figure 12 is the KOH solution process g-C with 5mol/L that embodiment 3.3 obtains 3n 4the process g-C obtained 3n 4the individual layer g-C obtained 3n 4the TEM figure of photocatalyst material.
Figure 13 be embodiment 5 obtain use 10%HNO 3process g-C 3n 4the g-C obtained 3n 4the TEM figure of photocatalyst material.
Figure 14 be embodiment 6 obtain with deionized water process g-C 3n 4the g-C obtained 3n 4the TEM figure of photocatalyst material.
Figure 15 is the KOH solution process g-C with 0.5mol/L that embodiment 7 obtains 3n 4the g-C obtained 3n 4the TEM figure of photocatalyst material.
Below in conjunction with the drawings and the specific embodiments, explanation is further explained to the present invention.
Embodiment
Embodiment 1.1:
Under room temperature, take 0.0526gg-C 3n 4, in agate mortar, be ground to powdery, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), join the HNO that 30ml mass concentration is 65% 3in, leave standstill 24h after stirring, use centrifuge tube intermittent supersound process 3h in 65 DEG C of water-bath medium frequencys ultrasonic apparatus that is 40000Hz after again stirring, being washed to pH is 6.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 80 DEG C, namely 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 the electron diffraction of any position all can occur six-membered ring structure, 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 0.0507gg-C 3n 4, in agate mortar, be ground to powdery, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), join the HNO that 30ml mass concentration is 50% 3in, leave standstill 24h after stirring, after again stirring at 60 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is 6, dries after being ground to powder, and it is even to add 50ml absolute ethyl alcohol and stirring, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 80 DEG C, namely 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 figure of this material as shown in Figure 5.
Embodiment 1.3:
Under room temperature, take 0.0571gg-C 3n 4, in agate mortar, be ground to powdery, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), join the HNO that 30ml mass concentration is 32% 3in, after stirring leave standstill 24h, after again stirring at 65 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is 6.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 60 DEG C, namely obtain the g-C of individual layer 3n 4.This individual layer g-C 3n 4interatomic distance is approximately 0.35nm, and the electron diffraction of any position all can occur six-membered ring structure, and thickness is approximately 0.334nm, and size is greatly between 700nm ~ 5um.The TEM figure of this material as shown in Figure 6.
Embodiment 2.1:
Under room temperature, take 0.0525gg-C 3n 4powdery is ground in agate mortar, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), joining 30ml mass concentration is in the HAc of 99.5%, 24h is left standstill after stirring, after again stirring at 80 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is after 6.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 80 DEG C, namely obtain the g-C of individual layer 3n 4, its thickness is 0.35nm, and size is greatly between 5um ~ 20um.The TEM figure of this monolayer material as shown in Figure 7.
Embodiment 2.2:
Under room temperature, take 0.0546gg-C 3n 4powdery is ground in agate mortar, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), joining 30ml mass concentration is in the HAc of 60%, 24h is left standstill after stirring, after again stirring at 65 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is after 6.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 70 DEG C, namely obtain the g-C of individual layer 3n 4, its thickness is 0.35nm, and size is greatly between 10um ~ 25um.The TEM figure of this monolayer material as shown in Figure 8.
Embodiment 2.3:
Under room temperature, take 0.0552gg-C 3n 4powdery is ground in agate mortar, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), joining 30ml mass concentration is in the HAc of 50%, 24h is left standstill after stirring, after again stirring at 65 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is after 6.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 80 DEG C, namely obtain the g-C of individual layer 3n 4, its thickness is 0.35nm, and size is greatly between 10um ~ 20um.The TEM figure of this monolayer material as shown in Figure 9.
Embodiment 3.1:
Under room temperature, take 0.0567gg-C 3n 4powdery is ground in agate mortar, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), joining 30ml concentration is in the KOH solution of 1mol/L, 24h is left standstill after stirring, after again stirring at 60 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is 8.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 80 DEG C, namely obtain the g-C of individual layer 3n 4, its thickness is 0.35nm, and size is greatly between 10um ~ 20um.The TEM figure of this monolayer material as shown in Figure 10.
Embodiment 3.2:
Under room temperature, take 0.0587gg-C 3n 4powdery is ground in agate mortar, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), joining 30ml concentration is in the KOH solution of 3mol/L, 24h is left standstill after stirring, after again stirring at 65 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is 8.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 80 DEG C, namely obtain the g-C of individual layer 3n 4, its thickness is 0.35nm, and size is greatly between 5um ~ 10um.The TEM figure of this monolayer material as shown in figure 11.
Embodiment 3.3:
Under room temperature, take 0.0578gg-C 3n 4powdery is ground in agate mortar, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), joining 30ml concentration is in the KOH solution of 5mol/L, 24h is left standstill after stirring, after again stirring at 80 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is 8.After oven dry is ground to powder, add 50ml absolute ethyl alcohol and stirring evenly, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 60 DEG C, namely obtain the g-C of individual layer 3n 4, its thickness is 0.35nm, and size is greatly between 10um ~ 25um.The TEM figure of this monolayer material 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, find in contriver:
(1) if use acid solution or alkaline solution to g-C 3n 4powder treatment and do not use supersound process time, or do not use acid solution or alkaline solution and directly to g-C 3n 4when powder adds water and carries out supersound process, then material color change is not obvious, and the stratiform g-C obtained 3n 4material is shown as multilayer and piles up block g-C 3n 4material.As embodiment 5, embodiment 6.
(2) if when the concentration of the acid solution added or alkaline solution is lower, g-C 3n 4powdered material color is also substantially unchanged, and just deposit to bottom centrifuge tube very soon in ultrasonication, ultrasonic effect is also not obvious, and product colour is darker.As embodiment 5 and embodiment 7.
(3) if the excessive concentration of the acid solution added or alkaline solution time, such as, add the H of excessive concentration in embodiment 4 2sO 4stratiform g-C after process 3n 4material color is too white, stirs rear and H 2sO 4dissolve each other, centrifugally can not get product.
Embodiment 4:
Under room temperature, take 0.0587gg-C 3n 4, in agate mortar, be ground to powdery, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), join the H that 30ml concentration is 98% 2sO 4in, faint yellow g-C in standing 24h process 3n 4become White Flocculus, become colorless after stirring transparence material, with H 2sO 4dissolve each other, centrifugally can not get spawn.
Embodiment 5:
Under room temperature, take 0.0504gg-C 3n 4, in agate mortar, be ground to powdery, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), join the HNO that 30ml mass concentration is 10% 3in, after stirring leave standstill 24h, after again stirring at 65 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is 6.Grinding is dried, the g-C obtained at 80 DEG C 3n 4be not individual layer, not quite, there is not considerable change in thickness yet for its lumpy sizes and untreated difference before.The TEM figure of this material as shown in figure 13.
Embodiment 6:
Under room temperature, take 0.0581gg-C 3n 4in agate mortar, be ground to powdery, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), join in the deionized water of 30ml, after stirring leave standstill 24h, after again stirring at 60 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h.Grinding is dried, unavailable g-C at 80 DEG C 3n 4be not individual layer, not quite, there is not considerable change in thickness yet for its lumpy sizes and untreated difference before.The TEM figure of this material as shown in figure 14.
Embodiment 7:
Under room temperature, take 0.0507gg-C 3n 4powdery is ground in agate mortar, after sieve degranulation footpath is greater than 0.106mm material (using 140 mesh sieve), joining 30ml concentration is in the KOH solution of 0.5mol/L, 24h is left standstill after stirring, after again stirring at 65 DEG C of water-bath medium frequencys be 40000Hz ultrasonic apparatus on intermittent supersound process 3h, being washed to pH is 8.Add 50ml absolute ethyl alcohol and stirring even, intermittent supersound process 3h.Use dehydrated alcohol centrifuge washing, dry grinding at 80 DEG C, the g-C obtained 3n 4be not individual layer, not quite, there is not considerable change in thickness yet for its lumpy sizes and untreated difference before.The TEM figure of this material as shown in figure 15.

Claims (2)

1. one kind has the individual layer g-C of monoatomic 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 4after being ground to powdery, join in acid solution or alkaline solution, leave standstill after stirring;
G-C 3n 40.001 is less than with the mass ratio of acid solution or alkaline solution;
Described acid solution is the H of mass concentration 20% ~ 50% 2sO 4the HNO of solution, mass concentration 32% ~ 65% 3solution, or 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;
Step 2: carry out supersound process after again being stirred by step 1 gained solution, to be precipitated completely after remove supernatant liquor, with deionized water rinsing to pH6 ~ 8; In described supersound process, ultrasonic temperature is 60 DEG C ~ 80 DEG C; Dry and pulverize last, joining in organic solvent and again carry out supersound process, to be precipitated completely after remove supernatant liquor;
Step 3: the g-C that step 2 is obtained 3n 4use dehydrated alcohol centrifuge washing, namely obtain the individual layer g-C with monoatomic thickness 3n 4.
2. the method for claim 1, is characterized in that, in described step 1, by block g-C 3n 4cross 140 mesh sieves after being ground to powdery, join in acid solution or alkaline solution.
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