CN108313989A - One type lamella shape nitrogenizes the preparation method and products obtained therefrom of carbosphere - Google Patents
One type lamella shape nitrogenizes the preparation method and products obtained therefrom of carbosphere Download PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses preparation method and products obtained therefrom that a type lamella shape nitrogenizes carbosphere, step is：Aqueous sucrose solution and nitrogenous organic precursor are uniformly mixed, hydro-thermal reaction is carried out at 170~190 DEG C, obtains the mixture of carbon ball and nitrogenous organic precursor, which is subjected to two-section calcining, obtains nitridation carbosphere.The present invention prepares simple, at low cost, product is made of several thin slices, pattern with class lamella, the microscopic appearance theoretically has the specific surface area of bigger compared with two-dimentional graphite phase carbon nitride material, it is conducive to provide more active sites and improves reactivity, nitrogenizing carbosphere can also be further compound with other materials, and application potential is shown in numerous areas such as photocatalysis.
Description
Technical field
The present invention relates to a kind of preparation methods of nitridation carbosphere, and in particular to a kind of pattern is special, class lamella shape nitrogen
The preparation method and products obtained therefrom for changing carbosphere, belong to technical field of semiconductor material preparation.
Background technology
Graphite phase carbon nitride is due to the two-dimensional slice structure similar with graphene, in recent years, causing people's
It constantly explores, and as a kind of catalysis material, is active in the fields such as photocatalysis and electro-catalysis.However, carbonitride is due to specific surface
Product is low, visible light absorption capacity is insufficient, and photo-generate electron-hole waits self-defects soon to recombination rate, largely all the time
On limit the application of carbonitride.In order to solve this problem, people have done a large amount of exploration.It has been found that changing carbonitride
Pattern, be realize carbonitride be modified effective means.A series of new shapes such as azotized carbon nano ball, nanotube, nano flower as a result,
Looks are synthesized, and applied to fields such as photocatalysis, electro-catalysis.
Control for carbonitride pattern, what people generally took is template.And in template, people generally use
Silica carries out nanosphere, nanotube as template, and the synthesis of the different morphologies such as thylakoid is comparative maturity and universal side
Method, the report that the new pattern synthesis of carbonitride is carried out using other templates are less.
Invention content
The object of the present invention is to provide a type lamella shape nitrogenize carbosphere preparation method and products obtained therefrom, this method with
For carbon ball as template, operating process is simple, at low cost, and gained nitridation carbosphere is formed by several thin slice self assemblies, has three-dimensional
The pattern of class lamella, pattern are special.
For the present invention using nitrogenous organic precursor, sucrose as raw material, water is solvent, and the carbon ball to be formed is dehydrated using sucrose as mould
Plate nitrogenizes carbosphere through being repeatedly thermally treated resulting in class lamella shape.The theoretical specific surface area ratio of the lamella shape pattern of this three-dimensional
The large specific surface area of traditional two-dimensional appearance provides new method for the synthesis of the new pattern of carbonitride, while this method has
Meaning is inspired well, can be used for the synthesis of other multiple materials.
Specific technical solution of the present invention is as follows：
A kind of preparation method of nitridation carbosphere, this approach includes the following steps：
（1）Aqueous sucrose solution and nitrogenous organic precursor are uniformly mixed, mixture is obtained；
（2）By step（1）Mixture carry out hydro-thermal reaction at 170~190 DEG C, detach reaction product, obtain carbon ball and nitrogenous have
The mixture of machine presoma；
（3）By step（2）Carbon ball and nitrogenous organic precursor mixture carry out two-section calcining, obtain nitridation carbosphere, it is described
The process of two-section calcining is：550 ~ 650 DEG C are warming up to, first time calcining is carried out under gas shield, is warming up to after natural cooling
It 500~540 DEG C, carries out calcining for second in air atmosphere, natural cooling.
In above-mentioned preparation method, using sucrose as carbon source, pass through step（2）Hydro-thermal reaction, sucrose is dehydrated to be formed containing micro-
The carbon ball in hole, and nitrogenous organic precursor is introduced into inside carbon ball during sucrose is dehydrated to form carbon ball, forms carbon ball
With the mixture of nitrogenous organic precursor.Pass through the control of subsequent calcination procedure, with the removal of carbon ball, nitrogenous organosilane precursor
Body occurs thermal polycondensation and forms carbonitride, forms the nitridation carbosphere of three-dimensional class lamella shape.
Further, above-mentioned steps（1）In, the mass ratio of nitrogenous organic precursor and sucrose is 0.05 ~ 0.4:1.
Further, sucrose is in step（1）Mixture in a concentration of 0.5~2 mol/L.
Further, the nitrogenous organic precursor is melamine or dicyandiamide.
Further, hydro-thermal reaction carries out under closed environment.In general, the time of hydro-thermal reaction is 4~6 h.
Further, the present invention is calcined at twice to control the pattern of final products, and the purpose of calcining has two sides for the first time
Face：First, so that the carbon in hydrothermal product is fully carbonized；Second, so that carbon containing nitrogen organic precursor thermal polycondensation is formed graphite-phase nitridation
Carbon.The purpose of calcining is for the second time：In air atmosphere by the graphited carbon complete oxidation in microballoon, template removes to obtain stone
Black phase carbon nitride microballoon.Preferably, when calcining for the first time, 550 ~ 650 DEG C are risen to the heating rate of 1~5 DEG C/min, second
When secondary calcining, 500~540 DEG C are risen to the heating rate of 1~2 DEG C/min.Preferably, when calcining for the first time, 550 ~ 650
DEG C heat preservation 2-6 h, second when calcining, and 4~6h is kept the temperature at 500~540 DEG C.
Further, step（3）In, when calcining for the first time, carried out under nitrogen or inert gas shielding.
Gained nitridation carbosphere of the invention is formed by carbonitride thin slice self assembly, and the size for nitrogenizing carbosphere is that 2-20 is micro-
Rice.The SEM figures of products obtained therefrom are as shown in Figures 2 and 3, it can be seen from the figure that the microscopic appearance of gained nitridation carbosphere is similar to bacterium
Pleated.Also, lamella shows more fluffy state.Product pattern of the present invention is special, the theoretical specific surface area ratio of the pattern
The large specific surface areas such as two-dimensional nanometer rods.Therefore, made from the above method nitrogenize carbosphere also the scope of the present invention it
It is interior.
For the present invention using nitrogenous organic precursor, sucrose as raw material, water is solvent, is by being dehydrated the carbon ball to be formed with sucrose
Template, the nitridation carbosphere special through being repeatedly thermally treated resulting in pattern.This method is simple and practicable, and cheap, repeatability
It is good, it is convenient for industrialized production.And this method has inspiration meaning, can be used for the synthesis of other multiple materials.Gained nitrogen of the invention
To change carbosphere to be made of carbonitride thin slice, shows more fluffy class lamella shape, the pattern is special, great novelty, such
Lamella shape three-dimensional appearance theoretically has the specific surface area of bigger compared with traditional two-dimentional carbon nitride material, is conducive to provide more
More active sites improves reactivity, which can also carry out effective compound, further rush with other substances
Into the separation and transfer of photoproduction electron hole pair, application potential is shown in numerous areas such as photocatalysis.
Description of the drawings
Fig. 1 is the XRD diagram that class lamella shape prepared by embodiment 1 nitrogenizes carbosphere.
Fig. 2 is the scanning electron microscope that class lamella shape prepared by embodiment 1 nitrogenizes carbosphere（SEM）Photo.
Fig. 3 is the scanning electron microscope that class lamella shape prepared by embodiment 2 nitrogenizes carbosphere（SEM）Photo.
Fig. 4 is the scanning electron microscope of nitridation carbosphere prepared by comparative example 1（SEM）Photo.
Fig. 5 is the scanning electron microscope of carbonitride sample prepared by comparative example 2（SEM）Photo.
Fig. 6 is the scanning electron microscope of carbonitride sample prepared by comparative example 3（SEM）Photo.
Specific implementation mode
Below by embodiment, the present invention will be further elaborated, it should be appreciated that, following the description merely to
It explains the present invention, its content is not defined.
Embodiment 1
20.5 g sucrose are dissolved in 40 ml deionized waters by 1.1, are made into 1.5 M（That is mol/L, similarly hereinafter）Sucrose solution.
1.2., 2 g melamines are added to the solution of step 1.1,0.5 h of stirring to melamine is uniformly dispersed.
1.3. the liquid of 40 ml steps 1.2 is transferred in 50 ml reaction kettles, 190 DEG C of 6 h of confined reaction, is centrifuged
Separation, obtains the mixture of carbon ball and melamine.
1.4. by step 1.3 resulting product with deionized water centrifuge washing multiple, naturally dry.
1.5. 1.4 products therefrom of above-mentioned steps is subjected to first time calcining under the protection of argon gas, with 1 DEG C/min
Heating rate be heated to 550 DEG C, 4 h are kept the temperature, later with stove natural cooling.
1.6., step 1.5 gained sample is carried out to second in air atmosphere to calcine, with the heating rate of 1 DEG C/min
It rises to 500 DEG C and keeps the temperature 4 h, obtain final products.
Fig. 1 is the XRD diagram of products obtained therefrom, and as can be seen from the figure thus obtained microsphere is graphite phase carbon nitride.Fig. 2 is gained production
The stereoscan photograph of product, it can be seen from the figure that about 5~20 microns of products obtained therefrom size, product is by carbonitride thin slice from group
It fills, is microballoon, microscopic appearance is class lamella shape, and lamella is in soft fluffy state.
Embodiment 2
27.3 g sucrose are dissolved in 40 ml deionized waters by 2.1, are made into the sucrose solution of 2 M.
2.2., 2 g melamines are added to the solution of step 2.1,0.5 h of stirring to melamine is uniformly dispersed.
2.3. the liquid of 40 ml steps 2.2 is transferred in 50 ml reaction kettles, 190 DEG C of 6 h of confined reaction, is centrifuged
Separation, obtains carbon ball/melamine mixture.
2.4. by step 2.3 resulting product with deionized water centrifuge washing multiple, naturally dry.
2.5. 2.4 products therefrom of above-mentioned steps is subjected to first time calcining under the protection of argon gas, with 1 DEG C/min
Heating rate be heated to 550 DEG C, 4 h are kept the temperature, later with stove natural cooling.
2.6. sample step 2.5 obtained carries out second and calcines in air atmosphere, with the heating speed of 1 DEG C/min
Rate rise to 500 DEG C and keep the temperature 4 h, obtain nitridation carbosphere, retouch electromicroscopic photograph as shown in figure 3, its by several thin slice self assemblies and
At pattern is class lamella shape, and size is in 5 ~ 15 microns.
Embodiment 3
13.7 g sucrose are dissolved in 40 ml deionized waters by 3.1, are made into the sucrose solution of 1 M.
3.2., 2 g melamines are added to the solution of step 3.1,0.5 h of stirring to melamine is uniformly dispersed.
3.3. the liquid of 40 ml steps 3.2 is transferred in 50 ml reaction kettles, 190 DEG C of 6 h of confined reaction, is centrifuged
Separation, obtains carbon ball/melamine mixture.
3.4. by step 3.3 resulting product with deionized water centrifuge washing multiple, naturally dry.
3.5. the product of the gained of above-mentioned steps 3.4 is subjected to first time calcining under the protection of argon gas, with 1 DEG C/
The heating rate of min is heated to 550 DEG C, 4 h is kept the temperature, later with stove natural cooling.
3.6. sample step 3.5 obtained carries out second and calcines in air atmosphere, with the heating speed of 1 DEG C/min
Rate rises to 500 DEG C and keeps the temperature 4 h, obtains nitridation carbosphere.It is class lamella shape that gained, which nitrogenizes carbosphere, and size is about 12 ~ 20 micro-
Rice.
Embodiment 4
6.8 g sucrose are dissolved in 40 ml deionized waters by 4.1, are made into the sucrose solution of 0.5 M.
4.2. 2g melamines are added in the solution of step 4.1,0.5 h of stirring to melamine is uniformly dispersed.
4.3. the liquid of 40 ml steps 4.2 is transferred in 50 ml reaction kettles, 190 DEG C of 6 h of confined reaction, is centrifuged
Separation, obtains carbon ball and melamine mixture.
4.4. by step 4.3 products obtained therefrom with deionized water centrifuge washing multiple, naturally dry.
4.5. 4.4 products therefrom of above-mentioned steps is subjected to first time calcining under the protection of argon gas, with 1 DEG C/min
Heating rate be heated to 550 DEG C, 4 h are kept the temperature, later with stove natural cooling.
4.6. sample step 5 obtained carries out second and calcines in air atmosphere, with the heating rate of 1 DEG C/min
It rises to 500 DEG C and keeps the temperature 4 h, obtain nitridation carbosphere.It is class lamella shape that gained, which nitrogenizes carbosphere, and size is 20 microns.
Embodiment 5
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：Melamine is replaced with into dicyandiamide.
Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 10 ~ 15 microns.
Embodiment 6
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：Prepare carbon ball and melamine mixture
When, in 170 DEG C of 6 h of confined reaction.Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size
About 5 ~ 10 microns.
Embodiment 7
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：The program of two-section calcining is：To wash,
Under the protection of argon gas, 550 are heated to the heating rate of 3 DEG C/min with melamine mixture for carbon ball after drying
DEG C carry out first time calcining, keep the temperature 4 h, later with stove natural cooling.Then it carries out calcining for second in air atmosphere, with 1
DEG C/heating rate of min rises to 500 DEG C and keeps the temperature 4 h, final nitridation carbosphere is obtained, pattern is similar with Fig. 2, for class
Lamella shape, carbonitride Microsphere Size are about 10 ~ 15 microns.
Embodiment 8
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：When calcining for the first time, heating rate 5
℃/min.Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 10 ~ 15 microns
Embodiment 9
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：Temperature when calcining for the first time is 600
℃.Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 5-15 microns.
Embodiment 10
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：Temperature when calcining for the first time is 650
℃.Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 5 ~ 10 microns.
Embodiment 11
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：Time when calcining for the first time is 2 h.
Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 10 ~ 15 microns.
Embodiment 12
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：Time when calcining for the first time is 6 h.
Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 8 ~ 15 microns.
Embodiment 13
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：Temperature when second of calcining is 520
℃.Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 10 ~ 15 microns.
Embodiment 14
20.5 g sucrose are dissolved in 40 ml deionized waters by 14.1, are made into the sucrose solution of 1.5 M.
14.2., 2g melamines are added to the solution of step 14.1,0.5 h of stirring to melamine is uniformly dispersed.
14.3. the liquid of 40 ml steps 14.2 is transferred in 50 ml reaction kettles, 190 DEG C of 6 h of confined reaction are obtained
To carbon ball/melamine mixture.
14.4. by step 14.3 products obtained therefrom with deionized water centrifuge washing multiple, naturally dry.
14.5. 14.4 products therefrom of above-mentioned steps is subjected to first time calcining under the protection of argon gas, with 1 DEG C/
The heating rate of min is heated to 550 DEG C, 4 h is kept the temperature, later with stove natural cooling.
14.6. sample step 14.5 obtained carries out second and calcines in air atmosphere, with the heating of 1 DEG C/min
Rate rises to 540 DEG C and keeps the temperature 4 h, obtains final products.Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape,
Carbonitride Microsphere Size is about 5 ~ 15 microns.
Embodiment 15
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：When second of calcining, heating rate 2
℃/min.Gained carbonitride microballoon pattern is similar with Fig. 2, is class lamella shape, carbonitride Microsphere Size is about 10 ~ 15 microns.
Embodiment 16
Class lamella shape, which is prepared, according to the method for embodiment 1 nitrogenizes carbosphere, unlike：When second of calcining, in air atmosphere
Under with the heating rate of 2 DEG C/min rise to 500 DEG C and keep the temperature 6 h.Gained carbonitride microballoon pattern is similar with Fig. 2, is class bacterium
Pleated, carbonitride Microsphere Size are about 10 ~ 15 microns.
Comparative example 1
Nitridation carbon products are prepared according to the method for embodiment 1, unlike：2 g sucrose are dissolved in 40 ml deionized waters, are made into
2 g melamines are added in the solution sucrose solution of 0.1 M, are dispersed with stirring uniformly.Final gained carbonitride pattern is as schemed
Shown in 4, it is the bead of 30 ~ 40 microns of diameter, is no longer lamella shape.It can thus be seen that sucrose and nitrogenous organic precursor
Proportioning, concentrations on product pattern have a major impact.
Comparative example 2
Nitridation carbon products are prepared according to the method for embodiment 1, unlike：When preparing carbon ball with melamine mixture,
160 DEG C of 6 h of confined reaction.Final gained carbonitride is not as shown in figure 5, products obtained therefrom has microballoon appearance.It can thus be seen that
Hydrothermal reaction condition has a major impact product morphology.
Comparative example 3
Nitridation carbon products are prepared according to the method for embodiment 1, unlike：By carbon ball and melamine mixture merely through a step
Calcining, program are as follows：The carbon ball washed, dried and melamine mixture are calcined in air atmosphere, with 1 DEG C/
The heating rate of min rises to 500 DEG C and keeps the temperature 4 h.Final gained carbonitride is as shown in fig. 6, without special appearance.Thus may be used
To find out, calcinating system has a major impact product morphology.
Comparative example 4
Nitridation carbon products are prepared according to the method for embodiment 1, unlike：When calcining for the first time, with the heating of 10 DEG C/min
Speed is heated to 550 DEG C, keeps the temperature 4 h；When second of calcining, rises to 500 DEG C with the heating rate of 5 DEG C/min and keep the temperature 4
h.Finally it is not collected into sample.It can thus be seen that heating rate has a major impact product morphology.
Comparative example 5
Nitridation carbon products are prepared according to the method for embodiment 1, unlike：When calcining for the first time, under the protection of argon gas, with 1
DEG C/heating rate of min is heated to 700 DEG C, 4 h are kept the temperature, later with stove natural cooling.When second of calcining, in air gas
Under atmosphere, rises to 500 DEG C with the heating rate of 1 DEG C/min and keep the temperature 4 h.Sample is not collected into after secondary clacining.It is possible thereby to
Find out, calcination temperature has a major impact product morphology.
Comparative example 6
Nitridation carbon products are prepared according to the method for embodiment 1, unlike：Sucrose is replaced with into glucose.Final gained nitridation
Carbon does not show special appearance.It can thus be seen that different carbon source has a major impact product morphology.
Claims (10)
1. a kind of preparation method of nitridation carbosphere, it is characterized in that including the following steps：
（1）Aqueous sucrose solution and nitrogenous organic precursor are uniformly mixed, mixture is obtained；
（2）By step（1）Mixture carry out hydro-thermal reaction at 170~190 DEG C, detach reaction product, obtain carbon ball and nitrogenous have
The mixture of machine presoma；
（3）By step（2）Carbon ball and nitrogenous organic precursor mixture carry out two-section calcining, obtain nitridation carbosphere, it is described
The process of two-section calcining is：550 ~ 650 DEG C are warming up to, first time calcining is carried out under gas shield, is warming up to after natural cooling
It 500~540 DEG C, carries out calcining for second in air atmosphere, natural cooling.
2. preparation method according to claim 1, it is characterized in that：Step（1）In, the matter of nitrogenous organic precursor and sucrose
Amount is than being 0.05 ~ 0.4:1；Sucrose is in step（1）Mixture in a concentration of 0.5~2 mol/L.
3. preparation method according to claim 1 or 2, it is characterized in that：The nitrogenous organic precursor be melamine or
Dicyandiamide.
4. preparation method according to claim 1, it is characterized in that：Step（2）In, the time of hydro-thermal reaction is 4~6 h.
5. preparation method according to claim 1, it is characterized in that：Step（3）In, for the first time calcine when, with 1~5 DEG C/
The heating rate of min rises to 550 ~ 650 DEG C, and when calcining for the second time, 500~540 are risen to the heating rate of 1~2 DEG C/min
℃。
6. preparation method according to claim 1 or 5, it is characterized in that：Step（3）In, when calcining for the first time, 550 ~
650 DEG C of heat preservation 2-6 h, when calcining for the second time, 4~6 h are kept the temperature at 500~540 DEG C.
7. according to the preparation method described in claim 1,4,5 or 6, it is characterized in that：Step（2）In, hydro-thermal reaction is in closed loop
It is carried out under border；Step（3）In, when calcining for the first time, carried out under nitrogen or inert gas shielding.
8. according to the preparation method described in any one of claim 1-7, it is characterized in that：It is thin by carbonitride that gained nitrogenizes carbosphere
Piece self assembly forms, and the size for nitrogenizing carbosphere is 2-20 microns.
9. the preparation method according to claim 1 or 8, it is characterized in that：Gained nitrogenizes the microscopic appearance of carbosphere similar to bacterium
Pleat.
10. nitrogenizing carbosphere made from the preparation method according to the nitridation carbosphere described in any one of claim 1-9.
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| CN110002414A (en) * | 2019-03-22 | 2019-07-12 | 张家港市东大工业技术研究院 | A kind of preparation method of nitride porous carbon nanotube |
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