CN105836801A - Three-dimensional porous NbS2 nano-material, and preparation method and application thereof - Google Patents
Three-dimensional porous NbS2 nano-material, and preparation method and application thereof Download PDFInfo
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a three-dimensional porous NbS2 nano-material, and a preparation method and application thereof. The preparation method comprises the following steps: putting niobium pentachloride powder into an open container A, then covering a part of the open mouth of the open container A with carbon fiber paper and putting the open container A in a high-temperature zone of a three-temperature-zone tubular furnace; weighing sulfur powder which is two times of the mole number of niobium pentachloride, putting the sulfur powder in an open container B and putting the open container B in a low-temperature zone of the three-temperature-zone tubular furnace; and heating the high-temperature zone of the three-temperature-zone tubular furnace to 500 to 700 DEG C at a heating rate of 10 DEG C/min under the condition that an airflow velocity is 100 sccm H2/Ar (15% of hydrogen) and maintaining the temperature for 20 min so as to eventually obtain the NbS2 nano-material. According to the invention, the carbon fiber paper is directly used as a substrate and an NbS2 nanoflake grows on the substrate through a CVD method; and the nanoflake can be directly used for an electrode material applied to hydrogen production through high-efficiency electrolysis, does not need any conductive agent and binder and has efficient catalysis performance and good cycle performance.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related to a kind of three-dimensional porous NbS2Nano material and preparation method thereof and
Application.
Background technology
Hydrogen is considered as to solve the one of energy resource consumption challenge in future as a kind of cleaning, continuable alternative fuel
Individual solution likely, therefore, producing and storing of hydrogen is the hydrogen energy source study hotspot that utilizes field.Wherein, electricity with
And PhotoelectrochemicalMethod Method decomposition water in acidic electrolyte bath is the main method producing hydrogen, but the method needs to use noble metal platinum
As catalyst, although platinum has fabulous catalytic capability, but high cost and low reserves seriously hinder its actual application.
To this end, design and synthesize a kind of advanced person material replace platinum become study hotspot.Up to now, a lot of nano materials success
Synthesize and be proved to the candidate material that can react as electrocatalytic hydrogen evolution, such as MoS2, CoS2, CoSe2, NiS2, FeP, MoSe2
Deng.But still there is activity and the problem of less stable compared with platinum in above-mentioned catalysis material.Therefore, earth deposit money is prepared
Source is abundant, activity is high, the catalysis material of good stability is still a problem demanding prompt solution.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of three-dimensional porous NbS2Nano material and preparation method thereof and should
With, the NbS obtained by the method2Nanometer sheet preparation is simple, can be directly used for high-efficient electrolytic water hydrogen manufacturing electrode material, it is not necessary to appoint
What conductive agent and binding agent.
The present invention takes techniques below scheme to reach described purpose:
1, a kind of three-dimensional porous NbS2Nano material, preparation method step includes: first take a certain amount of Columbium pentachloride. powder
Put in open-top receptacle A, then cover the mid portion of open-top receptacle A with carbon fiber paper and open-top receptacle A is placed on three
The high-temperature region of temperature-area tubular furnace；Weigh sulfur powder by the twice of Columbium pentachloride. molal quantity and sulfur powder is positioned in open-top receptacle B, with
Time open-top receptacle B is placed on the low-temperature space that three-temperature-zone diamond heating band is wound around, the high-temperature region of tube furnace is at 100sccm H2/
Under Ar (15% hydrogen) air velocity, it is warmed up to 500-700 DEG C with the heating rate of 10 DEG C/min, under 500-700 DEG C of high temperature
Keep 20 minutes, finally prepare NbS2Nano material.
Preferably, described NbS2Nano material is NbS2Nanometer sheet.
Preferably, the high-temperature region of described three-temperature-zone tube furnace is at 100sccm H2Under/Ar (15% hydrogen) air velocity, with
The heating rate of 10 DEG C/min is warmed up to 550 DEG C.
2, above-mentioned three-dimensional porous NbS2The preparation method of nano material, comprises the steps: first to take a certain amount of phosphoric
Niobium powder is put in open-top receptacle A, then covers the mid portion of open-top receptacle A with carbon fiber paper and is put by open-top receptacle A
Put the high-temperature region at three-temperature-zone tube furnace；Weigh sulfur powder by the twice of Columbium pentachloride. molal quantity and sulfur powder is positioned over open-top receptacle
In B, open-top receptacle B being placed on the low-temperature space that three-temperature-zone diamond heating band is wound around simultaneously, the high-temperature region of tube furnace exists
100sccm H2Under/Ar (15% hydrogen) air velocity, it is warmed up to 500-700 DEG C with the heating rate of 10 DEG C/min, at 500-
Keep 20 minutes under 700 DEG C of high temperature, finally prepare NbS2Nano material.
Preferably, described open-top receptacle A and B is porcelain boat.
Preferably, the area of described carbon fiber paper is 9 square centimeters.
3, above-mentioned three-dimensional porous NbS2Nano material application in electrocatalytic hydrogen evolution.
For electrode material, huge specific surface area can provide substantial amounts of active reaction sites, improves material
Specific capacity；And appearance structure has loose structure and is beneficial to reduce electrolyte ion diffusion path, improve diffusion rate.But have
The nano material of high-specific surface area is mostly powder body material, generally requires and suppress on a current collector equably during application, can not keep away
The electrocatalytic hydrogen evolution that organic bond is to improve its firmness contacted with collector and conventional at present can be used anti-with exempting from
The electrode material electric conductivity answered is poor, and electron transfer rate is relatively slow, also needs to mix with some conductive agents, this process during compacting
The part specific surface area not only allowing active material is lost, and reduces material property, also makes electrode production process more loaded down with trivial details.
In order to solve the problems referred to above, the present invention is directly with carbon fiber paper as substrate, fine at carbon by chemical vapour deposition technique
NbS is grown in dimension paper substrates2Nanometer sheet (NbS2NF/CFP), it is thus achieved that there is the NbS of high-specific surface area2Active material, end form
Integral polarizing electrode, is applied to electrocatalytic hydrogen evolution reaction.
The beneficial effects of the present invention is: the present invention, directly with carbon fiber paper as substrate, is existed by chemical vapour deposition technique
NbS is grown in carbon fiber paper substrate2Nanometer sheet (NbS2NF/CFP), this nanometer sheet is possible not only to improve the electricity of electrochemical reaction
Sub-transfer rate, huge surface area additionally provides more effective active reaction site, it is possible to utilize NbS greatly2
Nanometer sheet active material；It addition, directly improve electron transmission speed with carbon fiber paper for base material, can be directly used for efficiently
Water electrolysis hydrogen production electrode material, it is not necessary to any conductive agent and binding agent, greatly simplifies technique prepared by electrode, has saved one-tenth
This.
It addition, NbS of the present invention2Nanometer sheet has flaky nanometer structure and three-dimensional porous structure, on the one hand can increase
Add the transfer velocity of electronics, on the other hand effectively buffer the mechanical stress to structure in hydrogen generation process, therefore, the present invention
The sulfuration niobium nanometer sheet provided has relatively low liberation of hydrogen take-off potential (～178mV), less Tafel slope (41mV/dec)
And good long-time stability (lower 16 hours reaction after current density of overpotential-850mV is up to about 400mA/cm2), simultaneously
Have efficient catalytic performance and good cycle performance concurrently.
Chemical vapour deposition technique (CVD) preparation condition that the present invention uses is controlled, and the sample crystallinity deposited is high, and
Depositing homogeneous, beneficially material possess good chemical property；Furthermore, experiment condition of the present invention is simple, accurate to experimental apparatus
Degree requires low, simple to operate.
Accompanying drawing explanation
In order to make the purpose of the present invention, technical scheme and beneficial effect clearer, the present invention provides drawings described below, needs
Illustrate, NbS2NF/CFP represents carbon fiber paper substrate NbS2Nanometer sheet, CFP represents only carbon fiber paper, and Pt is platinum:
The NbS that Fig. 1 carbon fiber paper surface is formed2The SEM figure of nanometer sheet；
The NbS that Fig. 2 carbon fiber paper surface is formed2TEM figure, illustration is respectively electronogram and Fourier transformation figure；
Fig. 3 NbS2The XRD thing phase phenogram of nanometer sheet sample；
Fig. 4 NbS2The element Surface scan figure of nanometer sheet sample: be followed successively by NbS from a-d figure2The SEM of NF/CFP energy-spectrum scanning
C, Nb and the S distribution diagram of element of region and respective regions；
Fig. 5 NbS2The linear scanning curve chart of NF/CFP sample；
Fig. 6 NbS2The Tafel curve figure of NF/CFP sample；
Fig. 7 NbS2NF/CFP constant voltage steady testing figure；
Fig. 8 carbon fiber paper lay position view.
Detailed description of the invention
Below the preferred embodiments of the present invention are described in detail.The experiment side of unreceipted actual conditions in embodiment
Method, generally according to normal condition or according to the condition proposed by manufacturer.
Embodiment 1
NbS2The preparation method of nanometer sheet, comprises the following steps:
(1) take a certain amount of Columbium pentachloride. powder and put into aluminium oxide porcelain boat, clean carbon fiber paper is cut into 3cm × 3cm
Sheet covers live porcelain boat mid portion (as shown in Figure 8)；This porcelain boat is placed on the high-temperature region of three-temperature-zone tube furnace；
(2) weigh sulfur powder by the twice of Columbium pentachloride. molal quantity and sulfur powder is positioned in another porcelain boat, simultaneously by porcelain boat
It is placed on the low-temperature space that three-temperature-zone diamond heating band is wound around；
(3) high-temperature region of three-temperature-zone tube furnace is at 100sccm H2Under/Ar (15% hydrogen) air velocity, 10 DEG C/min's
Heating rate is warmed up to 550 DEG C, 550 DEG C of high-temperature process 20 minutes, finally prepares sulfuration niobium nanometer sheet.
Embodiment 2
Step with embodiment 1, difference be the high-temperature process temperature in step (3) be 500 DEG C.
Embodiment 3
Step with embodiment 1, difference be the high-temperature process temperature in step (3) be 600 DEG C.
Embodiment 4
Step with embodiment 1, difference be the high-temperature process temperature in step (3) be 650 DEG C.
Embodiment 5
Step with embodiment 1, difference be the high-temperature process temperature in step (3) be 700 DEG C.
Comparative example 1
In order to get rid of the carbon fiber paper (CFP) impact on experimental result, the present invention has done blank, and step is as follows:
A, the thin slice that clean carbon fiber paper is cut into 3cm × 3cm are laid on aluminium oxide porcelain boat；
B, porcelain boat is put into the high-temperature region of three-temperature-zone tube furnace, at 100sccm H2/ Ar (15% hydrogen) air velocity
Under, the heating rate of 10 DEG C/min is warmed up to 550 DEG C, rear 550 DEG C of high-temperature process 20 minutes.
Comparative example 2
In order to the catalytic hydrogen evolution performance of the sample embodiment 1 prepared with current commercialization platinum contrasts, the present invention exists
Testing the catalytic performance of commercialization platinum under identical conditions, concrete electrode preparation process is as follows:
Business-like Pt/C (20wt%) is sprayed to (the same embodiment of area load amount on carbon fiber paper by spraying method
1 is identical), after vacuum drying, it is used as integration catalysis electrode, enters test.
One, graphical analysis
1, the sample of embodiment 1 gained is carried out sem analysis, as it is shown in figure 1, it can be seen that carbon fiber paper is
It is sticked together by binding agent is random by a plurality of carbon fiber, finally constitutes a three-dimensional loose structure.Carbon fiber
Diameter is about 5 μm, and every carbon fiber is by NbS2Nanometer sheet wraps uniformly, NbS2The thickness of nanometer sheet is nanoscale, is difficult to thoroughly
Cross SEM measurement to draw.Additionally, there is a little NbS2Nanometer sheet agglomerates into microsphere and is distributed in NbS2In nanometer sheet.Therefore, carbon is utilized
Fiber, as base material, improves the electric conductivity of material；NbS at carbon fiber surrounding growth2Nanometer sheet improves active matter
The specific surface area of matter, and the loose structure formed is conducive to the diffusion of hydrogen and the holding of structure and morphology.
2, the sample of embodiment 1 gained is carried out tem analysis, as in figure 2 it is shown, from the TEM figure of low power it can be seen that
NbS2Nanometer sheet is to be piled up by monolayer or which floor nanometer sheet to form；The NbS prepared is can be seen that through electronic diffraction collection of illustrative plates2
Nanometer sheet belongs to monocrystalline system；Under the Fourier transformation figure of high power TEM and corresponding region is general, NbS2Crystal structure belong to six sides
Crystallographic system layer structure.The NbS prepared under this experimental technique is described2Purity is high.
3, the sample of embodiment 1 gained is carried out XRD material phase analysis, as it is shown on figure 3, it can be seen that carbon fiber
The diffraction maximum of some C of paper disappears or weakens, and NbS is described2Nanometer sheet is grown in around carbon fiber equably, and NbS2's
Diffraction maximum peak value and PDF standard card fit like a glove.
4, the sample of embodiment 1 gained is carried out element distribution analysis, as shown in Figure 4, it can be seen that this material
In really containing C, Nb, S these three element, and further illustrate Nb and S element and be evenly distributed in around carbon fiber.
Two, performance test
By the sample that obtains, (active area is 0.5cm2, politef adhesive tape is wound around redundance) and directly as work
Electrode, platinized platinum is as auxiliary electrode, and saturated calomel electrode is reference electrode, and electrolyte is the sulfuric acid solution of 0.5M, reference electrode
Standardization formula is E (RHE)=E (SCE)+0.240V.Linear scanning curve test scope is-0.65V～-0.1V, scanning speed
Degree is 5mV/s, at room temperature (23 ± 1 DEG C), the Hydrogen Evolution Performance of test sample.
1, embodiment 1, comparative example 1 and 2 are carried out linear scanning, as it is shown in figure 5, test result such as table 1.
Table 1 embodiment 1 drives overpotential required under electric current density
| Electric current density | 10mA/cm2 | 20mA/cm2 | 50mA/cm2 |
| Embodiment 1 | 178mV | 184mV | 193mV |
From figure 5 it can be seen that Pt/C electrode presents fabulous Hydrogen Evolution Performance close to 0, embodiment 1 is prepared
NbS2NF/CFP, after activating through certain time, also presents preferable Hydrogen Evolution Performance；And by test, carbon fiber paper does not has
There is electrocatalysis characteristic, thus can obtain, NbS2Hydrogen Evolution Performance superior for NF/CFP is not affected by base material carbon fiber paper.
2, Fig. 6 is the NbS prepared by the method for the present invention2The Tafel curve figure of NF/CFP sample, according to the test of Fig. 6
As a result, calculating embodiment 1, the slope of comparative example 1 and 2 according to Tafel formula (η=b logj+a), result of calculation is such as
Table 2.
Table 2 Tafel slope result of calculation, unit: mV/dec
| Embodiment | Embodiment 1 | Comparative example 1 | Comparative example 2 |
| Tafel slope | 40 | 101 | 31 |
3, embodiment 1 best for performance is carried out constant voltage steady testing, as it is shown in fig. 7, it can be seen that at head
In the constant high overpotential (-850mV) steady testing of individual 2h, electric current density presents ascendant trend, and then after 6h, electric current density is stable
At about 400mA/cm-2Although, the ensuing trend presenting reduction for several hours, but it is also stabilized in more than this numerical value, present
Preferably stability.
Above-described is only the preferred embodiment of the present invention, it is noted that for a person skilled in the art,
On the premise of without departing from present configuration, it is also possible to make some deformation and improvement, as prepared NbS by this method2Nanometer
Line, NbS2Nanometer rods, NbS2Nanometer film etc., these also should be considered as protection scope of the present invention, and these are all without affecting the present invention
The effect implemented and practical applicability.
Finally illustrate, preferred embodiment above only in order to technical scheme to be described and unrestricted, although logical
Cross above preferred embodiment the present invention to be described in detail, it is to be understood by those skilled in the art that can be
In form and it is made various change, without departing from claims of the present invention limited range in details.
Claims (7)
1. a three-dimensional porous NbS2Nano material, it is characterised in that preparation method step includes: first take a certain amount of phosphoric
Niobium powder is put in open-top receptacle A, then covers the mid portion of open-top receptacle A with carbon fiber paper and is put by open-top receptacle A
Put the high-temperature region at three-temperature-zone tube furnace；Weigh sulfur powder by the twice of Columbium pentachloride. molal quantity and sulfur powder is positioned over open-top receptacle
In B, open-top receptacle B being placed on the low-temperature space that three-temperature-zone diamond heating band is wound around simultaneously, the high-temperature region of tube furnace exists
100sccm H2Under/Ar (15% hydrogen) air velocity, it is warmed up to 500-700 DEG C with the heating rate of 10 DEG C/min, at 500-
Keep 20 minutes under 700 DEG C of high temperature, finally prepare NbS2Nano material.
The three-dimensional porous NbS of one the most according to claim 12Nano material, it is characterised in that described NbS2Nano material
For NbS2Nanometer sheet.
The three-dimensional porous NbS of one the most according to claim 12Nano material, it is characterised in that described three-temperature-zone tube furnace
High-temperature region at 100sccm H2Under/Ar (15% hydrogen) air velocity, it is warmed up to 550 DEG C with the heating rate of 10 DEG C/min.
4. the three-dimensional porous NbS described in any one of claims 1 to 32The preparation method of nano material, it is characterised in that include as
Lower step: first take a certain amount of Columbium pentachloride. powder and put in open-top receptacle A, then cover open-top receptacle A with carbon fiber paper
Mid portion and open-top receptacle A is placed on the high-temperature region of three-temperature-zone tube furnace；Weigh by the twice of Columbium pentachloride. molal quantity
Sulfur powder is also positioned in open-top receptacle B by sulfur powder, and open-top receptacle B is placed on the low of three-temperature-zone diamond heating band winding simultaneously
Warm area, the high-temperature region of tube furnace is at 100sccm H2Under/Ar (15% hydrogen) air velocity, with the heating rate liter of 10 DEG C/min
Temperature to 500-700 DEG C, keeps 20 minutes under 500-700 DEG C of high temperature, finally prepares NbS2Nano material.
Three-dimensional porous NbS the most according to claim 42The preparation method of nano material, it is characterised in that described uncovered appearance
Device A and B is porcelain boat.
Three-dimensional porous NbS the most according to claim 52The preparation method of nano material, it is characterised in that described carbon fiber
The area of paper is 9 square centimeters.
7. the three-dimensional porous NbS described in any one of claims 1 to 32Nano material application in electrocatalytic hydrogen evolution.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108557896A (en) * | 2018-05-02 | 2018-09-21 | 复旦大学 | A kind of preparation method of transition metal antimony sulfide |
| CN108585055A (en) * | 2018-05-25 | 2018-09-28 | 复旦大学 | A kind of Transition Metals V sulfide M V2S4Preparation method |
| CN108642517A (en) * | 2018-04-16 | 2018-10-12 | 肇庆市华师大光电产业研究院 | A method of utilizing Chinese photinia wood growing high density boundary molybdenum disulfide nano material |
| CN110093625A (en) * | 2019-04-25 | 2019-08-06 | 浙江大学 | A kind of application of liquid phase removing curing niobium nanometer sheet |
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| CN1413910A (en) * | 2002-11-27 | 2003-04-30 | 南开大学 | Transition metal sulfied nano-pipe and preparation process and its application |
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| CN102923777A (en) * | 2012-11-08 | 2013-02-13 | 镇江中孚复合材料有限公司 | Preparation method of six-square-piece shaped selenium doping disulfide niobium |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642517A (en) * | 2018-04-16 | 2018-10-12 | 肇庆市华师大光电产业研究院 | A method of utilizing Chinese photinia wood growing high density boundary molybdenum disulfide nano material |
| CN108557896A (en) * | 2018-05-02 | 2018-09-21 | 复旦大学 | A kind of preparation method of transition metal antimony sulfide |
| CN108585055A (en) * | 2018-05-25 | 2018-09-28 | 复旦大学 | A kind of Transition Metals V sulfide M V2S4Preparation method |
| CN108585055B (en) * | 2018-05-25 | 2020-12-18 | 复旦大学 | Transition metal vanadium sulfide MV2S4Preparation method of (1) |
| CN110093625A (en) * | 2019-04-25 | 2019-08-06 | 浙江大学 | A kind of application of liquid phase removing curing niobium nanometer sheet |
| CN110093625B (en) * | 2019-04-25 | 2020-05-08 | 浙江大学 | Application of liquid-phase stripped niobium disulfide nanosheet |
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| CN105836801B (en) | 2017-10-10 |
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