CN109019556A - It is a kind of to load the preparation method and gained carbon material for having the carbon material of metal oxide - Google Patents
It is a kind of to load the preparation method and gained carbon material for having the carbon material of metal oxide Download PDFInfo
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- CN109019556A CN109019556A CN201810890018.1A CN201810890018A CN109019556A CN 109019556 A CN109019556 A CN 109019556A CN 201810890018 A CN201810890018 A CN 201810890018A CN 109019556 A CN109019556 A CN 109019556A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
Abstract
The present invention provides a kind of preparation method and gained carbon material for loading and having the carbon material of metal oxide, and the preparation method includes: that (1) graphitization carbonitride is dried after mixing with aqueous metal salt；(2) products therefrom after step (1) drying is calcined, obtains the carbon material for loading and having metal oxide.The present invention also provides the carbon materials that the load obtained by the preparation method has metal oxide.This method realizes metal oxide in carbon surface uniform load, and the metal oxide particle that loads is uniform and size is small, avoids existing high temperature preparation method and is easy to appear the shortcomings that metallic particles is reunited to be graphitized carbonitride as template under cryogenic；And make to be graphitized carbonitride low-temperature denitrification formation conductive carbon material under cryogenic conditions, simultaneously oxidize metal object closely rivet in carbon material surface, when avoiding the preparation of existing other methods, metal oxide and the caducous problem of carbon material compound metallic particles.
Description
Technical field
The present invention relates to a kind of preparation methods and gained carbon material for loading and having the carbon material of metal oxide, belong to carbon materials
Expect technical field.
Background technique
The compound of metal oxide and carbon material is this kind of multiple because its unique physics and chemical property receive significant attention
It closes object and is widely used in the catalytic fields such as the energy storage fields such as lithium ion battery, sodium-ion battery and HER, OER, ORR, but letter
Just batch preparation is still puzzlement one of metal oxide and the widely applied bottleneck problem of compound of carbon material.Scientists
The method for reporting many compounds for preparing metal oxide and carbon material commonly includes hydro-thermal method, chemical vapor deposition
(CVD) method, chemical synthesis and mechanical attrition method etc., but wherein most preparation process it is complicated, it is expensive, by material from
Body structure limitation is serious.
Therefore it provides a kind of easy batch preparation load has the method for the carbon material of metal oxide to have become this field
The technical issues of urgent need to resolve.
Summary of the invention
In order to solve the above shortcomings and deficiencies, it is an object of the present invention to provide a kind of loads metal oxide
Carbon material preparation method.
Another object of the present invention, which also resides in, provides the preparation method system for the carbon material for having metal oxide by above-mentioned load
Standby obtained load has the carbon material of metal oxide.
In order to achieve the above objectives, on the one hand, the present invention provides a kind of preparation side for loading and having the carbon material of metal oxide
Method, wherein the preparation method includes:
(1) graphitization carbonitride is dried after mixing with aqueous metal salt；
(2) products therefrom after step (1) drying is calcined, obtains the carbon material for loading and having metal oxide.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, the mass ratio of graphitization carbonitride and metal nitrate described in step (1) is 1:1-10.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, metal salt described in step (1) includes metal nitrate.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, metal nitrate described in step (1) includes ferric nitrate, nickel nitrate, cobalt nitrate, zinc nitrate, magnesium nitrate, aluminum nitrate or nitric acid
One of copper or several combinations.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, drying temperature described in step (1) is 70-100 DEG C, time 10-12h.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, the temperature of calcining described in step (2) is 200-700 DEG C, time 10-120min.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, the temperature of calcining described in step (2) is 300-400 DEG C.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, in calcination process, metal oxide is generated in the case where temperature is lower than 290 DEG C, when temperature is 290-700 DEG C, metal oxidation
Object is catalyzed nitrogen-atoms, and then forms the carbon material for loading and having metal oxide.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, metal salt generates metal oxide (temperature is before 290 DEG C) after decomposing, and in g-C3N4One layer of fine and close gold of upper load
Belong to oxide skin(coating), the metal oxide and g-C3N4There are more contact sites, then with the promotion (290-700 of temperature
DEG C) metal oxide can be catalyzed nitrogen-atoms in connection and make the nitrogen-atoms from g-C3N4It falls off on skeleton, and then forms carbon
Material.
Specific embodiment according to the present invention, load of the invention have the preparation method of the carbon material of metal oxide
In, the graphitization carbonitride (g-C3N4) can be prepared using conventional method in that art.
On the other hand, the present invention also provides described load to have the preparation method of the carbon material of metal oxide to be prepared
Load have the carbon material of metal oxide, wherein the metal oxide uniform load is in the surface of carbon material, and the metal
Oxide is of uniform size, partial size 2-10nm, has the total weight of the carbon material of metal oxide for 100% with described load
Meter, the content of metal oxide are 60%-90%.
Specific embodiment according to the present invention has in the carbon material that the load has metal oxide with the load
The total weight of the carbon material of metal oxide is 100% meter, and the content of metal oxide is 70%-90%.
The load provided by the present invention has the preparation method of the carbon material of metal oxide to be graphitized carbonitride as mould
Plate, under cryogenic realize metal oxide carbon surface uniform load, and load metal oxide particle uniformly and
Size is small, avoids existing high temperature preparation method and is easy to appear the shortcomings that metallic particles is reunited；And make stone under cryogenic conditions
Inkization carbonitride low-temperature denitrification forms conductive carbon material, at the same oxidize metal object closely rivet in carbon material surface,
When avoiding the preparation of existing other methods, metal oxide and the caducous problem of carbon material compound metallic particles.
Detailed description of the invention
Figure 1A is scanning electron microscope (SEM) photograph (20.0 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 1
m)；
Figure 1B is scanning electron microscope (SEM) photograph (1.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 1
m)；
Fig. 2A is scanning electron microscope (SEM) photograph (40.0 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 2
m)；
Fig. 2 B is scanning electron microscope (SEM) photograph (5.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 2
m)；
Fig. 3 A is scanning electron microscope (SEM) photograph (20.0 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 3
m)；
Fig. 3 B is scanning electron microscope (SEM) photograph (2.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 3
m)；
Fig. 4 A is scanning electron microscope (SEM) photograph (20.0 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 4
m)；
Fig. 4 B is scanning electron microscope (SEM) photograph (2.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 4
m)；
Fig. 5 is scanning electron microscope (SEM) photograph (5.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 5
m)；
Fig. 6 A is scanning electron microscope (SEM) photograph (10.0 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 6
m)；
Fig. 6 B is scanning electron microscope (SEM) photograph (1.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 6
m)；
Fig. 7 A is scanning electron microscope (SEM) photograph (10.0 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 7
m)；
Fig. 7 B is scanning electron microscope (SEM) photograph (1.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 7
m)；
Fig. 8 A is scanning electron microscope (SEM) photograph (10.0 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 8
m)；
Fig. 8 B is scanning electron microscope (SEM) photograph (1.00 μ for the carbon material that load has metal oxide provided by the embodiment of the present invention 8
m)。
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now in conjunction in detail below
Embodiment carries out following detailed description to technical solution of the present invention, but should not be understood as the limit to enforceable range of the invention
It is fixed.
Embodiment 1
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into containing 14.5g nickel nitrate and 29g cobalt nitrate
In 300mL aqueous solution, after dry, move in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 310 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 12g can be obtained, that is, load the carbon material for having metal oxide, have metal with the load
The total weight of the carbon material of oxide is 100% meter, and the content of metal oxide is 70%, is denoted as NiCo2O4/C；Do not need through
Cross any subsequent processing.
Electron microscope analysis, electron microscope difference are scanned to the carbon material that the load obtained by the present embodiment has metal oxide
As illustrated in figures 1A and ib, it can be seen that from Figure 1A and Figure 1B；The load obtained by the present embodiment has the carbon of metal oxide
In material, fine and close metal oxide uniform load forms the structure for being similar to durian peel shape, and the gold in the surface of carbon material
It is of uniform size to belong to oxide, partial size 5-10nm.
Embodiment 2
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into the 300mL aqueous solution containing 29g cobalt nitrate, does
After dry, move in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 350 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 8g can be obtained, that is, load the carbon material for having metal oxide, have metal oxygen with the load
The total weight of the carbon material of compound is 100% meter, and the content of metal oxide is 60%, is denoted as Co3O4/C；It needs not move through and appoints
What subsequent processing.
Electron microscope analysis, electron microscope difference are scanned to the carbon material that the load obtained by the present embodiment has metal oxide
As shown in Figure 2 A and 2 B, it can be seen that from Fig. 2A and Fig. 2 B；The load obtained by the present embodiment has the carbon of metal oxide
In material, fine and close metal oxide uniform load is in the surface of carbon material, and the metal oxide is of uniform size, and partial size is
3-8nm。
Embodiment 3
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into the 300mL aqueous solution containing 20g ferric nitrate, does
After dry, move in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 310 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 8g can be obtained, that is, load the carbon material for having metal oxide, have metal oxygen with the load
The total weight of the carbon material of compound is 100% meter, and the content of metal oxide is 80%, is denoted as Fe3O4/C；It needs not move through and appoints
What subsequent processing.
Electron microscope analysis, electron microscope difference are scanned to the carbon material that the load obtained by the present embodiment has metal oxide
As shown in Fig. 3 A and Fig. 3 B, it can be seen that from Fig. 3 A and Fig. 3 B；The load obtained by the present embodiment has the carbon of metal oxide
In material, fine and close metal oxide uniform load is in the surface of carbon material, and the metal oxide is of uniform size, and partial size is
3-8nm。
Embodiment 4
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into the aqueous solution containing 14.5g nickel nitrate, it is dry
Afterwards, it moves in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 300 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 7g can be obtained, that is, load the carbon material for having metal oxide, have metal oxygen with the load
The total weight of the carbon material of compound is 100% meter, and the content of metal oxide is 60%, is denoted as NiO/C；It needs not move through any
Subsequent processing.
Electron microscope analysis, electron microscope difference are scanned to the carbon material that the load obtained by the present embodiment has metal oxide
As shown in fig. 4 a and fig. 4b, it can be seen that from Fig. 4 A and Fig. 4 B；The load obtained by the present embodiment has the carbon of metal oxide
In material, fine and close metal oxide uniform load is in the surface of carbon material, and the metal oxide is of uniform size, and partial size is
5-10nm。
Embodiment 5
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into the aqueous solution containing 20g copper nitrate, after dry,
It moves in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 350 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 10g can be obtained, that is, load the carbon material for having metal oxide, have metal with the load
The total weight of the carbon material of oxide is 100% meter, and the content of metal oxide is 75%, is denoted as CuO/C；It needs not move through and appoints
What subsequent processing.
Electron microscope analysis is scanned to the carbon material that the load obtained by the present embodiment has metal oxide, electron microscope is as schemed
Shown in 5, as can be seen from Figure 5；In the carbon material that the load obtained by the present embodiment has metal oxide, fine and close metal oxygen
Compound uniform load is in the surface of carbon material, and the metal oxide is of uniform size, partial size 3-9nm.
Embodiment 6
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into the aqueous solution containing 8g magnesium nitrate and 29g cobalt nitrate
In, after dry, move in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 350 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 11g can be obtained, that is, load the carbon material for having metal oxide, have metal with the load
The total weight of the carbon material of oxide is 100% meter, and the content of metal oxide is 85%, is denoted as MgCo2O4/C；Do not need through
Cross any subsequent processing.
Electron microscope analysis, electron microscope difference are scanned to the carbon material that the load obtained by the present embodiment has metal oxide
As shown in Fig. 6 A and Fig. 6 B, it can be seen that from Fig. 6 A and Fig. 6 B；The load obtained by the present embodiment has the carbon of metal oxide
In material, fine and close metal oxide uniform load is in the surface of carbon material, and the metal oxide is of uniform size, and partial size is
4-10nm。
Embodiment 7
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into water-soluble containing 20g aluminum nitrate and 29g cobalt nitrate
In liquid, after dry, move in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 360 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 14g can be obtained, that is, load the carbon material for having metal oxide, have metal with the load
The total weight of the carbon material of oxide is 100% meter, and the content of metal oxide is 82%, is denoted as Al2Co6O12/C；It does not need
By any subsequent processing.
Electron microscope analysis, electron microscope difference are scanned to the carbon material that the load obtained by the present embodiment has metal oxide
As shown in figs. 7 a and 7b, it can be seen that from Fig. 7 A and Fig. 7 B；The load obtained by the present embodiment has the carbon of metal oxide
In material, fine and close metal oxide uniform load is in the surface of carbon material, and the metal oxide is of uniform size, and partial size is
2-8nm。
Embodiment 8
Present embodiments provide a kind of preparation method for loading and having the carbon material of metal oxide comprising following steps:
(1) 15g urea is placed in ceramic crucible, which is placed in Muffle furnace in 550 DEG C of holding 4h, is obtained
Faint yellow solid, as with the g-C of cavernous structure3N4；
(2) 5g step (1) resulting g-C is weighed3N4, it is added into the water containing 14.5g nickel nitrate and 29g cobalt nitrate
In solution, after dry, move in crucible；
(3) crucible that raw material is housed in step (2) is placed into Muffle furnace, in 700 DEG C of holding 10min of set temperature,
It then is naturally cooling to room temperature, product 10g can be obtained, that is, load the carbon material for having metal oxide, have metal with the load
The total weight of the carbon material of oxide is 100% meter, and the content of metal oxide is 90%, is denoted as NiCo2O4/C；Do not need through
Cross any subsequent processing.
Electron microscope analysis, electron microscope difference are scanned to the carbon material that the load obtained by the present embodiment has metal oxide
As shown in Fig. 8 A and Fig. 8 B, it can be seen that from Fig. 8 A and Fig. 8 B；The load obtained by the present embodiment has the carbon of metal oxide
In material, fine and close metal oxide uniform load is in the surface of carbon material, and the metal oxide is of uniform size, and partial size is
3-10nm。
Claims (10)
1. a kind of load the preparation method for having the carbon material of metal oxide, which is characterized in that the preparation method includes:
(1) graphitization carbonitride is dried after mixing with aqueous metal salt；
(2) products therefrom after step (1) drying is calcined, obtains the carbon material for loading and having metal oxide.
2. preparation method according to claim 1, which is characterized in that graphitization carbonitride and metal described in step (1)
The mass ratio of nitrate is 1:1-10.
3. preparation method according to claim 1 or 2, which is characterized in that metal salt described in step (1) includes metal nitre
Hydrochlorate.
4. preparation method according to claim 3, which is characterized in that the metal nitrate include ferric nitrate, nickel nitrate,
One of cobalt nitrate, zinc nitrate, magnesium nitrate, aluminum nitrate or copper nitrate or several combinations.
5. preparation method according to claim 1, which is characterized in that drying temperature described in step (1) is 70-100 DEG C,
Time is 10-12h.
6. preparation method according to claim 1, which is characterized in that the temperature of calcining described in step (2) is 200-700
DEG C, time 10-120min.
7. preparation method according to claim 6, which is characterized in that the temperature of calcining described in step (2) is 300-400
℃。
8. preparation method according to claim 6 or 7, which is characterized in that in calcination process, metal oxide is low in temperature
It is generated at 290 DEG C, when temperature is 290-700 DEG C, the metal oxide oxidation catalyst nitrogen-atoms, and then the formation load has gold
Belong to the carbon material of oxide.
9. the load that any one of the claim 1-8 load has the preparation method of the carbon material of metal oxide to be prepared has
The carbon material of metal oxide, which is characterized in that the metal oxide uniform load is in the surface of carbon material, and the metal oxygen
Compound is of uniform size, partial size 2-10nm, by it is described load have metal oxide carbon material total weight be 100% in terms of,
The content of metal oxide is 60%-90%.
10. according to claim 9 load the carbon material for having metal oxide, which is characterized in that have gold with the load
The total weight for belonging to the carbon material of oxide is 100% meter, and the content of metal oxide is 70%-90%.
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| CN109867265A (en) * | 2019-03-11 | 2019-06-11 | 江苏大学 | A method of the orderly metal oxide of macropore is prepared using Supramolecular self assembly |
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