CN109621998A - A kind of three-dimensional meso-hole carbon load molybdenum carbide and its preparation method and application - Google Patents
A kind of three-dimensional meso-hole carbon load molybdenum carbide and its preparation method and application Download PDFInfo
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Abstract
本发明属于纳米材料制备领域，公开了一种三维介孔碳负载碳化钼及其制备和应用。本发明将可溶性钼盐溶解在水中，然后加入有机物碳源和模板剂，调节溶液pH值到0～7.0，然后搅拌蒸干水分得到凝胶，凝胶进一步脱水得到干凝胶，在惰性气体或者还原气体气氛下，将干凝胶高温煅烧，有机物碳源碳化得到碳，且有机物碳源碳化过程产生的还原性物质能够将钼还原碳化得到纳米碳化钼，然后用稀酸浸泡除去即得目标产物。相比于块体碳化钼材料而言，三维介孔碳负载碳化钼具有导电的三维碳网络结构，更大的比表面积，更多的反应活性位点，且碳负载结构防止了碳化钼在高温煅烧时的团聚，因此三维介孔碳负载碳化钼具有优良的电催化性能。
The invention belongs to the field of nanomaterial preparation, and discloses a three-dimensional mesoporous carbon-supported molybdenum carbide and its preparation and application. In the present invention, soluble molybdenum salt is dissolved in water, then organic carbon source and template agent are added, the pH value of the solution is adjusted to 0-7.0, and then the water is evaporated to dryness by stirring to obtain a gel, and the gel is further dehydrated to obtain a dry gel. Under a reducing gas atmosphere, the dry gel is calcined at high temperature, and the organic carbon source is carbonized to obtain carbon, and the reducing substances generated during the carbonization of the organic carbon source can reduce and carbonize the molybdenum to obtain nano-molybdenum carbide, and then soak it with dilute acid to remove the target product. . Compared with the bulk molybdenum carbide material, the three-dimensional mesoporous carbon-supported molybdenum carbide has a conductive three-dimensional carbon network structure, a larger specific surface area, more reactive sites, and the carbon-supported structure prevents the molybdenum carbide from being exposed to high temperatures. agglomeration upon calcination, so the three-dimensional mesoporous carbon-supported molybdenum carbide has excellent electrocatalytic performance.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, in particular to a kind of three-dimensional meso-hole carbon load molybdenum carbide and its system
Preparation Method and application.
Background technique
With the development of water electrolysis hydrogen production technology, at low cost, efficient water electrolysis hydrogen production method is obtained, used in
The demand of electrode catalyst is to be more and more obvious.Since the noble metals such as Pt are at high cost as electrolysis water catalyst, the low spy of reserves
Point, developing the novel non-precious metal catalyst of one kind just becomes the hot spot studied now, wherein transition metal carbides exist
Extensive concern is caused in the research process of electrolysis water.Transition metal carbide is by being embedded in carbon in transition metal lattice
Atom simultaneously forms chemical bond and is formed.Compared with its base metal and metal oxide, transition metal carbide can be shown
Far different physics and chemical property are shown.Transition metal carbide not only has high-melting-point, high rigidity and high tensile,
Possess high conductance and thermal conductivity simultaneously.It has recently been demonstrated that transition metal carbide shows the catalysis similar to noble metal
Characteristic, and these unique catalysis characteristics and its electronic structure and crystal structure are closely related.For molybdenum carbide, due to carbon
Change the unique interstitial compound structure of molybdenum, carbon atom can cause the expansion of molybdenum lattice, make after being embedded into molybdenum atom dot matrix
The distance between molybdenum atom is obtained to increase.The increase of this metal-metal atomic distance can cause molybdenum atom d energy band to be shunk,
So as to cause the increase of the d energy band density of molybdenum.On the other hand, in molybdenum carbide the s-p track of carbon and the d track of molybdenum can generate it is miscellaneous
Change, generated hydridization d track can appear similar to the electronic structure of precious metals pt.According to band theory, the electricity of d energy band
Sub- property can influence the absorption and activation of reactant significantly.Therefore molybdenum carbide is expected to obtain the catalysis spy for being similar to precious metals pt
Property, there is important researching value.
Carbon material has the potentiality as efficient stable HER catalyst due to its resistance to acid and alkali, high conductivity the features such as, so
And (hydrogen adsorbs Gibbs free energy Δ GH* ,~1.3eV to weak hydrogen adsorption capacity；And excellent HER catalyst often have~
The Δ GH* value of 0eV) cause it to embody extremely slow catalytic kinetics.And carbon carried metal/alloy catalyst (active site
It is considered as being referred to as " armor " catalyst due to its excellent catalytic activity and stability on the carbon-coating on surface) in recent years
It has received widespread attention.Therefore, exploitation carbon composite catalytic agent is of great significance to the HER catalyst for developing eka-platinium performance.Separately
On the one hand, there is the nano material of three-dimensional (3-D) reticular structure to receive much attention since it is multi-functional, such as big specific surface
An important factor for product, three-dimensional porous structure, big specific surface area and three-dimensional porous structure are influence composite material electrocatalysis characteristics,
They are conducive to the absorption of proton, the exposure of active site, flowing of electrolyte etc..
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of three-dimensional meso-hole
The preparation method of carbon load molybdenum carbide.
Another object of the present invention is to provide the three-dimensional meso-hole carbon load molybdenum carbide of above method preparation.
Still a further object of the present invention is to provide the application of above-mentioned three-dimensional meso-hole carbon load molybdenum carbide.
The purpose of the present invention is realized by following proposal:
A kind of preparation method of three-dimensional meso-hole carbon load molybdenum carbide, comprising the following steps:
(1) it prepares gel: soluble molybdenum salt is dissolved in water, add organic carbon source and template, it is uniformly mixed
Mixed solution, the pH value for adjusting mixed solution is 0~7, and being stirred under heating makes mixed solution be evaporated to obtain gel, by gel into one
Step thermal dehydration obtains xerogel；
(2) it prepares three-dimensional meso-hole carbon load molybdenum carbide: xerogel obtained by step (1) being ground uniformly, is put into tube furnace
High temperature cabonization restores, and inert gas or reducing gas is passed through in reaction process, after reaction, by products therefrom acid soak
Molybdenum carbide is loaded up to target product three-dimensional meso-hole carbon.
Soluble molybdenum salt described in step (1) includes but is not limited to ammonium molybdate, molybdenum chloride, sodium molybdate etc.；
Organic carbon source described in step (1) includes but is not limited to citric acid, diammonium hydrogen citrate, glucose, dicyan two
Ammonia, cyanamide etc..
Template described in step (1) is silica or magnesia, the partial size of the template is 10~
1000nm；
Template described in step (1) is preferably added in the form of aqueous dispersions, the moisture of the template
The mass concentration of template is preferably 40% in dispersion liquid；
The dosage of soluble molybdenum salt, organic carbon source and template described in step (1) meets: organic carbon source and solubility
The mass ratio of molybdenum salt is (0.5~10): 1；The mass ratio of organic carbon source and template is (0.2~5): 1.
Preferably, the dosage of soluble molybdenum salt, organic carbon source and template described in step (1) meets: organic carbon source
Mass ratio with soluble molybdenum salt is (2.5~4): 1；The mass ratio of organic carbon source and template is (1~3): 1.
Water described in step (1) is intended only as reaction medium, therefore only to need it that can be completely dissolved added for its dosage
The soluble molybdenum salt and organic carbon source entered.
Heating stirring described in step (1) refer to be heated to 60~80 DEG C be stirred to react 4~for 24 hours, stirring is to make
It is adequately mixed between raw material, therefore the mixing speed of this field routine can be realized；
Further thermal dehydration described in step (1) refer to be heated to 100~200 DEG C reaction 4~for 24 hours；
The reduction of high temperature cabonization described in step (2) refers in 600~1200 DEG C of 2~12h of carbonizing reduction；
Inert gas described in step (2) or reducing gas include but is not limited to nitrogen, argon gas, hydrogen, argon gas/hydrogen
Gas gaseous mixture；
Acid described in step (2) be concentration be 2~8wt% hydrofluoric acid, one of hydrochloric acid；
Immersion described in step (2) refers to 1~48h of immersion, preferably 2~8h of immersion；
Do not indicate that temperature refers both to carry out at room temperature in the present invention, the room temperature is 20~30 DEG C；
A kind of three-dimensional meso-hole carbon load molybdenum carbide prepared by the above method.
Application of the three-dimensional meso-hole carbon load molybdenum carbide that the above method is prepared as electrocatalysis material, especially as
Application of the electrocatalysis material in catalytic water decomposing hydrogen-production.
Mechanism of the invention are as follows:
Soluble molybdenum salt is dissolved in water by the present invention first, and organic matter carbon source such as citric acid, hydrogen citrate is then added
Diammonium, glucose, dicyan diamino, cyanamide etc. add template silica or magnesia, stir evenly, use ammonium hydroxide
Solution ph is adjusted between 0~7.0, promotes organic matter carbon source molecule with molybdenum element in conjunction with, at this time in 60~80 DEG C of stirrings steamings
Solid carbon dioxide gets gel, is then further dehydrated gel at 100~200 DEG C and obtains xerogel, in inert gas or reduction
Under gas atmosphere, xerogel is reacted at 600~1200 DEG C, in high-temperature burning process, organic matter carbon source is carbonized to obtain carbon, and has
Molybdenum can be restored carbon by the reducing substances such as carbon monoxide, carbon dioxide, methane and the carbon that machine object carbon source carbonisation generates
Change obtains nano silicon carbide molybdenum, therefore, obtains silica (magnesia)/molybdenum carbide/carbon composite after reaction, then will
Silica (magnesia), which is impregnated to remove with diluted hydrofluoric acid (dilute hydrochloric acid), loads molybdenum carbide (two up to target product three-dimensional meso-hole carbon
Silica or magnesia are used as pore-creating sacrifice agent).For block is carbonized molybdenum material, three-dimensional meso-hole carbon loads molybdenum carbide tool
There is conductive three-dimensional carbon network structure, there are bigger specific surface area, more reactivity sites, and carbon support structures prevent
Reunion of the molybdenum carbide in high-temperature calcination, therefore three-dimensional meso-hole carbon load molybdenum carbide has excellent electrocatalysis characteristic.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) present invention realizes the controlledly synthesis of three-dimensional meso-hole carbon load molybdenum carbide.
(2) the three-dimensional meso-hole carbon load molybdenum carbide structure novel that the present invention synthesizes, and electrocatalytic decomposition water hydrogen manufacturing performance is steady
It is fixed.
(3) this simple process is controllable, can quickly amplify industrialization.
Detailed description of the invention
Fig. 1 is the XRD diagram that three-dimensional meso-hole carbon prepared by embodiment 1 loads molybdenum carbide；
Fig. 2 is the XRD diagram that three-dimensional meso-hole carbon prepared by embodiment 2 loads molybdenum carbide；
Fig. 3 is the XRD diagram that three-dimensional meso-hole carbon prepared by embodiment 3 loads molybdenum carbide；
Fig. 4 is the SEM figure that three-dimensional meso-hole carbon prepared by embodiment 3 loads molybdenum carbide；
Fig. 5 is the polarization curve that three-dimensional meso-hole carbon prepared by embodiment 3 loads molybdenum carbide；
Fig. 6 is the SEM figure that three-dimensional meso-hole carbon prepared by embodiment 4 loads molybdenum carbide；
Fig. 7 is the TEM figure that three-dimensional meso-hole carbon prepared by embodiment 4 loads molybdenum carbide；
Fig. 8 is the polarization curve that three-dimensional meso-hole carbon prepared by embodiment 4 loads molybdenum carbide；
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Polarization curve test method is as follows in the present embodiment:
Electrode preparation: firstly, glass-carbon electrode (GCE) polishing powder (Al for being 3mm by diameter2O3) sanding and polishing, and use second
Pure and mild deionized water cleaned standby seam.Secondly, weighing 4mg catalyst in centrifuge tube, it is added in 750m L deionized water, 250 μ L
Ethyl alcohol and 30 μ L Nafion solutions, ultrasonic disperse is uniform, pipettes the 5 above-mentioned solution of μ L and drips on GCE, and irradiates under infrared lamp
It is dry.The load capacity for being computed catalyst is 0.285mg cm-2。
Electro-chemical test: all electrochemical datas measure on CHI 660E electrochemical workstation, and electrolyte is
1.0M KOH solution, uses N2Purification.In typical three electrode tests system, coated graphite rod electrrode is to have catalyst to electrode
GCE be working electrode, Ag/AgCl electrode be reference electrode.After catalyst is stable in the electrolyte, with 5m V s-1Scanning
Rate carries out polarization curve (LSV) test, and all current potentials use reversible hydrogen electrode (RHE) to indicate, reduction formula:
ERHE=EAg/AgCl+0.059pH+Eθ Ag/AgCl
Eθ Ag/AgCl=0.198V
Embodiment 1
A kind of preparation method of three-dimensional meso-hole carbon load molybdenum carbide of the present embodiment, specific preparation process is as follows:
In deionized water by soluble ammonium molybdate 6.0g dissolution, 15.0g diammonium hydrogen citrate is then added, dissolution is complete
40g silica dispersions (dioxide-containing silica 40wt%, 15 ± 5nm of silica partial size) is added afterwards, then is adjusted with ammonium hydroxide
The pH=6.0 of above-mentioned solution, then stirring is evaporated 12 hours and obtains gel at 70 DEG C, then by gel further at 200 DEG C
Dehydration obtains xerogel in 12 hours, and xerogel is ground uniformly, 900 DEG C carbonizing reduction 2 hours, reaction process in tube furnace are put into
In be passed through 5% (v/v) H2/ Ar gaseous mixture is stirred 4 hours with excessive 4.0wt% hydrofluoric acid dips after reaction, filtering,
Molybdenum carbide is loaded after natural drying up to target product three-dimensional meso-hole carbon.
The XRD diagram of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in Figure 1, three-dimensional meso-hole carbon loads molybdenum carbide
XRD test feature peak be 36.9 °, 42.8 °, 62.7 ° with 75.3 °, respectively correspond (111) of α-MoC, (200), (220)
With (311) crystal face.24.9 ° of characteristic peak corresponds to (002) crystal face of graphitized carbon.
Molybdenum carbide is loaded to three-dimensional meso-hole carbon prepared by the present embodiment by scanning electron microscope to detect, and is found
It illustrates that the present embodiment successfully synthesizes the target product of three-dimensional meso-hole with apparent order meso-hole structure.
Embodiment 2
A kind of preparation method of three-dimensional meso-hole carbon load molybdenum carbide of the present embodiment, specific preparation process is as follows:
In deionized water by soluble sodium molybdate 6.0g dissolution, 20.0g cyanamide is then added, is added after dissolving completely
40g silica dispersions (dioxide-containing silica 40wt%, 15 ± 5nm of silica partial size) adjust above-mentioned solution with nitric acid
PH=7, then stirring is evaporated 12 hours and obtains gel at 70 DEG C, and gel is then put into tube furnace 700 DEG C of carbonizations also
It is 2 hours former, 5% (v/v) H is passed through in reaction process2/ Ar gaseous mixture, after reaction with excessive 2.0wt% hydrofluoric acid dips
Stirring 8 hours, filtering load molybdenum carbide after natural drying up to target product three-dimensional meso-hole carbon.
The XRD diagram of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in Fig. 2, three-dimensional meso-hole carbon loads molybdenum carbide
XRD test feature peak be 36.9 °, 42.8 °, 62.7 ° with 75.3 °, respectively correspond (111) of α-MoC, (200), (220)
With (311) crystal face.24.9 ° of characteristic peak corresponds to (002) crystal face of graphitized carbon.
Molybdenum carbide is loaded to three-dimensional meso-hole carbon prepared by the present embodiment by scanning electron microscope to detect, and is found
It illustrates that the present embodiment successfully synthesizes the target product of three-dimensional meso-hole with apparent order meso-hole structure.
Embodiment 3
A kind of preparation method of three-dimensional meso-hole carbon load molybdenum carbide of the present embodiment, specific preparation process is as follows:
Soluble ammonium molybdate 6.0g is dissolved in deionized water, 18.0g dicyan diamino is then added, is added after dissolving completely
Enter 40g silica dispersions (dioxide-containing silica 40wt%, 15 ± 5nm of silica partial size), is adjusted with nitric acid above-mentioned molten
The pH=4.5 of liquid, then stirring is evaporated 12 hours and obtains gel at 80 DEG C, and gel is further then dehydrated 12 at 180 DEG C
Hour obtains xerogel, and xerogel is ground uniformly, 900 DEG C carbonizing reduction 2 hours in tube furnace is put into, is passed through in reaction process
10% (v/v) H2/ Ar gaseous mixture is stirred 2 hours with excessive 4.0wt% hydrofluoric acid dips after reaction, and filtering is naturally dry
Molybdenum carbide is loaded after dry up to target product three-dimensional meso-hole carbon.
The XRD diagram of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in figure 3, three-dimensional meso-hole carbon loads molybdenum carbide
XRD test feature peak be 34.3 °, 37.7 °, 39.3 °, 52.1 °, 61.5 °, 69.4 °, 72.4 °, 74.6 ° with 75.5 °, point
β-Mo is not corresponded to2(100) of C, (002), (101), (102), (110), (103), (200), (112) and (201) crystal face.
24.9 ° of characteristic peak corresponds to (002) crystal face of graphitized carbon.
The SEM figure of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in figure 4, three-dimensional meso-hole carbon loads molybdenum carbide
Composite material has apparent order meso-hole structure.
The polarization curve of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in figure 5, three-dimensional meso-hole carbon loads carbon
Changing the electric current that molybdenum generates is -10mA cm-2When corresponding bias be -193mV.
Embodiment 4
A kind of preparation method of three-dimensional meso-hole carbon load molybdenum carbide of the present embodiment, specific preparation process is as follows:
In deionized water by soluble ammonium molybdate 5.0g dissolution, 20.0g citric acid is then added, is added after dissolving completely
40g silica dispersions (dioxide-containing silica 40wt%, 15 ± 5nm of silica partial size) adjust above-mentioned solution with ammonium hydroxide
PH=1.5, then stirring is evaporated 12 hours and obtains gel at 70 DEG C, then that gel is further small in 200 DEG C of dehydrations 12
When obtain xerogel, by xerogel grind uniformly, be put into 900 DEG C carbonizing reduction 4 hours in tube furnace, be passed through in reaction process
10% (v/v) H2/ Ar gaseous mixture is stirred 4 hours with excessive 4.0wt% hydrofluoric acid dips after reaction, and filtering is naturally dry
Molybdenum carbide is loaded after dry up to target product three-dimensional meso-hole carbon.
The SEM figure of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in fig. 6, three-dimensional meso-hole carbon loads molybdenum carbide
Composite material has apparent order meso-hole structure.
The TEM figure of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in fig. 7, the carbonization that three-dimensional meso-hole carbon loads
Molybdenum partial size about 2~4nm.
The polarization curve of the load molybdenum carbide of three-dimensional meso-hole carbon obtained by the present embodiment is as shown in figure 8, three-dimensional meso-hole carbon loads carbon
Changing the electric current that molybdenum generates is -10mA cm-2When corresponding bias be -167mV.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
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