CN107090586A - A kind of FeS2RGO composites, preparation method and applications - Google Patents
A kind of FeS2RGO composites, preparation method and applications Download PDFInfo
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- CN107090586A CN107090586A CN201710239742.3A CN201710239742A CN107090586A CN 107090586 A CN107090586 A CN 107090586A CN 201710239742 A CN201710239742 A CN 201710239742A CN 107090586 A CN107090586 A CN 107090586A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a kind of FeS2RGO composites, preparation method and applications.The FeS of the present invention2RGO composites are by the way that graphene oxide is dissolved in DMF, then the aqueous solution of Fe(NO3)39H2O and thioacetamide is sequentially added, is stirred overnight at a temperature of 85~95 DEG C, then passes through hydro-thermal reaction redox graphene, centrifugation, washing, it is lyophilized after, calcining under hydrogen is obtained；The FeS of the present invention2RGO composites can be used for electrocatalytic hydrogen evolution, because the cost of raw material is low, and preparation method is simple, and Hydrogen Evolution Performance is good, and catalyst stability is good, solve well now due to preparing hydrogen cost height, it is difficult to the problem of industrialization development.
Description
Technical field
The present invention relates to production hydrogen technical field, specifically, it is related to a kind of FeS2- RGO composites, preparation method and its
Using.
Background technology
The energy is the basic of human survival, is also the basic of national development.In the strategy of country, the energy often occupies ten
Point consequence, while which determining the depth and broadness of national development, also determines a national ups and downs.
Relative to the new renewable and clean energy resource such as solar energy, nuclear energy, hydrogen has that preparation condition is relatively easy, equipment dimension
The advantages such as shield is simple, environmental protection.Liberated heat is big when it burns, and product is water, free from environmental pollution, therefore, is used as one kind
Reproducible green energy resource, hydrogen is widely applied prospect by it, enters our visual field, regard hydrogen as novel energy
Instead of fossil fuel, the study hotspot of the world today is also become.Conventional method, which prepares hydrogen, mainly includes water-gas method and stone
Oil-breaking method etc..However, the hydrogen purity that these methods are prepared is relatively low, while need to consume substantial amounts of fossil feedstock, therefore,
Carry out hydrogen making by raw material of water, the new technology including photodissociation aquatic products hydrogen and electrolysis aquatic products hydrogen is obtaining the wide of people
General concern.Water electrolysis hydrogen production is that a kind of security is higher, the higher ripe hydrogen producing technology of efficiency, but in water electrolysis hydrogen production process
In, generally require to consume huge electric energy, therefore, how the research emphasis of water electrolysis hydrogen production is mainly reducing electrolytic energy now
Aspect, and as the most key water electrolysis hydrogen production catalyst used in electrolytic energy is reduced in water electrolysis hydrogen production, also it is natural into
The forward position studied for our times.
The selection of main efficiency catalyst when being to rely on electrolysis of electrolysis aquatic products hydrogen, one of them main condition is exactly
Need close to the absorption H with product+With reference to energy.And it is current, HER efficiency highest catalyst is Pt, and Pt only needs to very small
Absorption H+Combination can be with regard to reaction can be made, when it is electrolysed, overpotential is close to 0V.However, Pt is on earth
Content is but and its rare, and its content on the earth's crust is about 0.001~0.005mg/Kg.This directly results in anti-with Pt catalytic hydrogen evolutions
Answer cost higher.Therefore, developing a kind of cheap and with sustainability electrolysis water catalyst just becomes people's concern
Focus.At present, transition metal mainly includes transition metal phosphide, transition metal selenizing as electrolysis aquatic products hydrogen catalyst
Thing, carbide and transient metal sulfide etc..
In transient metal sulfide, CoS2, NiS2, FeS2, MoS2Deng transient metal sulfide, there is very strong electro-catalysis
Activity.With MoS2Exemplified by, it in recent years, has obtained very big development as the popular catalyst of electrolysis aquatic products hydrogen.
Chorkendorff breakthrough Journal of Sex Research shows MoS2The exposure of (010) and (100) face unsaturated Mo and S position be HER
Avtive spot.And basal plane (002) face is then its HER inertia site.Just because of this discovery, people put research emphasis
How in synthesis nano MoS2During on the exposure of maximum possible its avtive spot.For example, with rich end face position
The MoS of point2It can be realized by die version method using the orderly double helix face body mesh architecture with cavernous structure.2013,
Jin team is found that 1T-MoS first2Compare 2H-MoS2There are higher metallicity and Geng Gao HER catalytic activity, this is mainly
Because the former electric conductivity is more much higher than the latter.Chhowalla team is further discovered that 1T-MoS2Avtive spot
2H-MoS2Avtive spot it is different, it is predominantly located at basal plane.So our 1T-MoS enhancing catalytic activity2It is attributed to it i.e.
Avtive spot is added, the electric conductivity of catalyst is enhanced again.
Transient metal sulfide has special 3d valence electron shell structurres, and this characteristic brings excellent property to material
Energy.Such as WS2In terms of catalysis, lubricating utensil, battery manufacture, refractory material, pigment, optics and magnetic apparatus, have
Very strong practical value.And molybdenum sulfide and iron sulfide, as the more excellent material of property in transient metal sulfide, attracting
While people largely pay close attention to, it is also widely used for producing and lives central.Therefore, research cost is relatively low, better performances
Transition-metal catalyst has and its important meaning.
The content of the invention
In view of the above-mentioned problems, the present invention propose a kind of cheap composite elctro-catalyst preparation method and it urged in electricity
Change the application in terms of liberation of hydrogen.Described electrocatalytic hydrogen evolution material reduces cost in existing electrocatalysis material, reduces analysis
The overpotential of hydrogen, improves the stability of catalyst, enhances the performance of electro-catalysis system liberation of hydrogen.Cost of material is low, hydrogen evolution activity
Site is more and stability is stronger.
Technical scheme is specifically described as follows.
The present invention provides a kind of FeS2The preparation method of-RGO composites, is comprised the following steps that：
Graphene oxide is synthesized by Hummer first, then graphene oxide is dissolved in DMF, then sequentially added
The aqueous solution of Fe(NO3)39H2O and thioacetamide, is stirred overnight at a temperature of 85~95 DEG C, then by hydro-thermal reaction also
Former graphene oxide, centrifugation, washing, it is lyophilized after, finally calcine under hydrogen, produce FeS2- RGO composites；The oxygen
The mass ratio of graphite alkene, Fe(NO3)39H2O and thioacetamide is (3~7)：(60~80)：(140~160).
In the present invention, hydrothermal temperature is 175~185 DEG C；The hydro-thermal reaction time is 5~10 hours.
In the present invention, calcining heat is 590~610 DEG C；Calcination time is 2~4 hours.
The present invention also provides the FeS that a kind of above-mentioned preparation method is obtained2- RGO composites.FeS therein2In six sides
The form of shape is present, FeS2Average grain diameter in 600~700nm or so.
The present invention further provides a kind of above-mentioned FeS2The electrocatalytic hydrogen evolution application of-RGO composites in an acidic solution.
This
The electrocatalytic hydrogen evolution performance of invention is tested using following methods：
(1) 1mg FeS are weighed2- RGO composites are dissolved in 100 μ L 0.2-0.5wt% Nation solution, are surpassed
Sound is dispersed；Then scattered rear solution is drawn into 6-18 μ L on glass-carbon electrode, dried naturally；
(2) be passed through nitrogen and throw out air, sulfuric acid solution clean glass-carbon electrode electrode surface, then by glass-carbon electrode,
Ag/AgCl electrodes, platinum electrode connect electrochemical workstation, in an acidic solution the performance of test compound material electrocatalytic hydrogen evolution；
Overpotential is reduced, and Tafel curves increase, liberation of hydrogen works well.
Compared to the prior art, the beneficial effects of the present invention are：
Using the electrocatalytic hydrogen evolution material of the present invention in acid medium electrolysis water, liberation of hydrogen effect of the present invention is found by contrast
Well, hydrogen evolution activity site is more, and stability is preferable, cost is relatively low.
In the present invention, graphene oxide is a kind of new carbon of excellent performance, with higher specific surface area and
The abundant functional group in surface.FeS is loaded using graphene oxide2Nano-particle, can increase load capacity, be urged so as to improve electricity
Change the hydrogen evolution activity site of material.The characteristic being combined according to catalyst and carbon material, elctro-catalyst FeS2Load to oxygen reduction
On graphite alkene RGO, the overpotential during liberation of hydrogen can be reduced, strengthens stability, improves the activity of electrocatalytic hydrogen evolution.Profit
Liberation of hydrogen material is calcined with hydrogen, can make that graphene oxide is reduced more thoroughly, during electrolysis separates out hydrogen and need not first use
Carry out redox graphene, the amount of precipitation of hydrogen can be improved, further enhance the Hydrogen Evolution Performance of electrocatalysis material.It is molten in acidity
The performance of the composite electrocatalytic hydrogen evolution is measured in liquid, overpotential reduction, Tafel curves increase, liberation of hydrogen works well.
Brief description of the drawings
Fig. 1：A. the scanning electron microscope (SEM) photograph of the electrocatalytic hydrogen evolution material of the gained of embodiment 1；B. the polarization of Application Example 1 is bent
Line.C. the Tafel collection of illustrative plates of Application Example 1.
Fig. 2：A. the scanning electron microscope (SEM) photograph of the electrocatalytic hydrogen evolution material of the gained of embodiment 2；B. the polarization of Application Example 2 is bent
Line.C. the Tafel collection of illustrative plates of Application Example 2.
Fig. 3：A. the scanning electron microscope (SEM) photograph of the electrocatalytic hydrogen evolution material of the gained of embodiment 3；B. the polarization of Application Example 3 is bent
Line.C. the Tafel collection of illustrative plates of Application Example 3.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.
Various raw materials used, are commercially available unless otherwise specified in various embodiments of the present invention.
Embodiment 1
Raw material composition when preparing composite is as follows：
Graphene oxide 5mg
Fe(NO3)39H2O 72mg
Thioacetamide 145mg
N,N-dimethylformamide 16ml
The 5wt% μ L of Nation solution 8
98% concentrated sulfuric acid 13ml
Absolute ethyl alcohol is a little
Absolute methanol is a little
Surplus is distilled water
The preparation method of above-mentioned composite as follows：
Graphene oxide is synthesized by improved Hummer methods.Fe(NO3)39H2O is made into 0.2M solution, by sulphur
1M solution is made into for acetamide, then by graphene oxide ultrasonic dissolution in 8ml DMF, ferric nitrate and thioacetyl is added
Amine aqueous solution, stirs 24h at 90 DEG C, then cools down, centrifuges, and with water washing is distilled 3 times, removes unreacted raw material.Then again
DMF solution 5-10 hour of hydro-thermal inside water heating kettle is added, then is centrifuged, with water washing is distilled 3 times, finally, is fired under hydrogen
Burning obtains FeS2- RGO composites.Its pattern is as shown in Figure 1a.
Application Example 1
The product of embodiment 1 is ground, glassy carbon electrode surface is clean using 0.05 μm of alumina lap, remove
Residual sample, is rinsed well using second alcohol and water, dried.
(1) Nation solution 0.3wt% is matched somebody with somebody with absolute methanol.The above-mentioned composite dissolvings of 1mg are weighed to configure in 100 μ L
Nation solution in, dispersed two hours under ultrasound.Then the solution is drawn into 6-18 μ L on glass-carbon electrode again,
Naturally dry.
(2) above-mentioned 98% sulfuric acid solution is configured to 0.5M sulfuric acid solution, nitrogen is passed through and throws out air, with 0.5M sulphur
Acid solution cleans the electrode surface of glass-carbon electrode, and glass-carbon electrode, Ag/AgCl electrodes, platinum electrode then are connected into electrochemical operation
Stand, the performance (as shown in Figure 1 b) of the composite electrocatalytic hydrogen evolution is measured in an acidic solution, the Tafel of the elctro-catalyst is oblique
Rate is 63.46mV/decade (as illustrated in figure 1 c), and the electrocatalysis characteristic is than simple.
Embodiment 2
Raw material composition when preparing composite is as follows：
Graphene oxide 4mg
Fe(NO3)39H2O 72mg
Thioacetamide 150mg
N,N-dimethylformamide 16ml
The 5wt% μ L of Nation solution 8
98% concentrated sulfuric acid 13ml
Absolute ethyl alcohol is a little
Absolute methanol is a little
Surplus is distilled water
The preparation method of above-mentioned composite as follows：
Graphene oxide is synthesized by improved Hummer methods.Fe(NO3)39H2O is made into 0.2M solution, by sulphur
1M solution is made into for acetamide, then by graphene oxide ultrasonic dissolution in 10ml DMF, ferric nitrate and thio second is added
Amide solution, stirs 24h at 90 DEG C, then cools down, centrifuges, and with water washing is distilled 3 times, removes unreacted raw material.Then
DMF solution 5-10 hour of hydro-thermal inside water heating kettle is added, then is centrifuged, with water washing is distilled 3 times, finally, under hydrogen
Burning obtains FeS2- RGO composites.Its pattern is as shown in Figure 2 a.
Application Example 2
The product of embodiment 1 is ground, glassy carbon electrode surface is clean using 0.05 μm of alumina lap, remove
Residual sample, is rinsed well using second alcohol and water, dried.
(1) Nation solution 0.5wt% is matched somebody with somebody with absolute methanol.The above-mentioned composite dissolvings of 1mg are weighed to configure in 100 μ L
Nation solution in, dispersed two hours under ultrasound.Then the solution is drawn into 6-18 μ L on glass-carbon electrode again,
Naturally dry.
(2) above-mentioned 98% sulfuric acid solution is configured to 0.5M sulfuric acid solution, nitrogen is passed through and throws out air, with 0.5M sulphur
Acid solution cleans the electrode surface of glass-carbon electrode, and glass-carbon electrode, Ag/AgCl electrodes, platinum electrode then are connected into electrochemical operation
Stand, the performance (as shown in Figure 2 b) of the composite electrocatalytic hydrogen evolution is measured in an acidic solution, the Tafel of the elctro-catalyst is oblique
Rate is 59.59mV/decade (as shown in Figure 2 c).
Embodiment 3
Raw material composition when preparing composite is as follows：
Graphene oxide 4mg
Fe(NO3)39H2O 80mg
Thioacetamide 150mg
N,N-dimethylformamide 16ml
The 5wt% μ L of Nation solution 10
98% concentrated sulfuric acid 13ml
Absolute ethyl alcohol is a little
Absolute methanol is a little
Surplus is distilled water
The preparation method of above-mentioned composite as follows：
Graphene oxide is synthesized by improved Hummer methods.Fe(NO3)39H2O is made into 0.2M solution, by sulphur
1M solution is made into for acetamide, then by graphene oxide ultrasonic dissolution in 10ml DMF, ferric nitrate and thio second is added
Amide solution, stirs 24h at 90 DEG C, then cools down, centrifuges, and with water washing is distilled 3 times, removes unreacted raw material.Then
DMF solution 5-10 hour of hydro-thermal inside water heating kettle is added, then is centrifuged, with water washing is distilled 3 times, finally, under hydrogen
Burning obtains FeS2- RGO composites.Its pattern is as shown in Figure 3 a.
Application Example 3
The product of embodiment 1 is ground, glassy carbon electrode surface is clean using 0.05 μm of alumina lap, remove
Residual sample, is rinsed well using second alcohol and water, dried.
(1) Nation solution 0.5wt% is matched somebody with somebody with absolute methanol.The above-mentioned composite dissolvings of 1mg are weighed to configure in 100 μ L
Nation solution in, dispersed two hours under ultrasound.Then the solution is drawn into 6-18 μ L on glass-carbon electrode again,
Naturally dry.
(2) above-mentioned 98% sulfuric acid solution is configured to 0.5M sulfuric acid solution, nitrogen is passed through and throws out air, with 0.5M sulphur
Acid solution cleans the electrode surface of glass-carbon electrode, and glass-carbon electrode, Ag/AgCl electrodes, platinum electrode then are connected into electrochemical operation
Stand, the performance (as shown in Figure 3 b) of the composite electrocatalytic hydrogen evolution is measured in an acidic solution, the Tafel of the elctro-catalyst is oblique
Rate is 68.83mV/decade (as shown in Figure 3 c).
Claims (5)
1. a kind of FeS2The preparation method of-RGO composites, it is characterised in that comprise the following steps that：
Graphene oxide is synthesized by Hummer first, then graphene oxide is dissolved in DMF, nine water are then sequentially added
The aqueous solution of ferric nitrate and thioacetamide is closed, is stirred overnight at a temperature of 85~95 DEG C, then pass through hydro-thermal reaction oxygen reduction
Graphite alkene, centrifugation, washing, it is lyophilized after, finally calcine under hydrogen, produce FeS2- RGO composites；The oxidation stone
The mass ratio of black alkene, Fe(NO3)39H2O and thioacetamide is (3~7)：(60~80)：(140~160).
2. preparation method according to claim 1, it is characterised in that hydrothermal temperature is 175~185 DEG C；Hydro-thermal is anti-
It is 5~10 hours between seasonable.
3. preparation method according to claim 1, it is characterised in that calcining heat is 590~610 DEG C；Calcination time is 2
~4 hours.
4. the FeS that a kind of preparation method according to one of claims 1 to 3 is obtained2- RGO composites, it is characterised in that
FeS therein2Exist in hexagonal form, FeS2Average grain diameter in 600~700nm or so.
5. a kind of FeS according to claim 42The electrocatalytic hydrogen evolution application of-RGO composites in an acidic solution.
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Cited By (4)
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| CN107699919A (en) * | 2017-10-17 | 2018-02-16 | 上海应用技术大学 | Fe2‑1.5xMoxS2RGO hybrid catalysts and its preparation method and application |
| CN107761128A (en) * | 2017-11-10 | 2018-03-06 | 上海应用技术大学 | A kind of FeNiNC electrode materials, preparation method and applications |
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| CN111463439A (en) * | 2019-01-21 | 2020-07-28 | 中国科学院福建物质结构研究所 | Composite, bifunctional catalyst containing composite and electrochemical neutralization energy battery |
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| CN107699919A (en) * | 2017-10-17 | 2018-02-16 | 上海应用技术大学 | Fe2‑1.5xMoxS2RGO hybrid catalysts and its preparation method and application |
| CN107699919B (en) * | 2017-10-17 | 2019-07-23 | 上海应用技术大学 | Fe2-1.5xMoxS2- RGO hybrid catalyst and its preparation method and application |
| CN107761128A (en) * | 2017-11-10 | 2018-03-06 | 上海应用技术大学 | A kind of FeNiNC electrode materials, preparation method and applications |
| CN107761128B (en) * | 2017-11-10 | 2019-12-03 | 上海应用技术大学 | A kind of FeNiNC electrode material, preparation method and applications |
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| CN111463439A (en) * | 2019-01-21 | 2020-07-28 | 中国科学院福建物质结构研究所 | Composite, bifunctional catalyst containing composite and electrochemical neutralization energy battery |
| CN111463439B (en) * | 2019-01-21 | 2022-02-18 | 中国科学院福建物质结构研究所 | Composite, bifunctional catalyst containing composite and electrochemical neutralization energy battery |
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Application publication date: 20170825 |