CN106971849A - NiSe electrocatalysis materials and its production and use - Google Patents
NiSe electrocatalysis materials and its production and use Download PDFInfo
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- CN106971849A CN106971849A CN201710364305.4A CN201710364305A CN106971849A CN 106971849 A CN106971849 A CN 106971849A CN 201710364305 A CN201710364305 A CN 201710364305A CN 106971849 A CN106971849 A CN 106971849A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
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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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Abstract
The present invention discloses NiSe electrocatalysis materials and its production and use, and NiSe electrocatalysis materials are the hexagonal crystal shape of sheet, and interplanar distance is2 θ angles are to have stronger absworption peak at 35.8 °, 42.7 °, 45.3 °, 59.0 °, 61.9 °, 68.8 °, 69.1 °, 82.5 °, 83.1 °；Flock together in cotton-shaped pattern.The NiSe electrocatalysis materials that the present invention is prepared are to catalysis reduction I3 ‑Show excellent electro catalytic activity.They are used for DSSC (DSSCs) to obtaining preferable photoelectric transformation efficiency in electrode, 8.10% is reached as high as；Compared with standard Pt is the DSSCs performances (PCE=7.82%) to electrode, excellent electro catalytic activity is shown.
Description
Technical field
The present invention relates to the drilling fluid in petroleum drilling engineering.It is used for deep-well, horizontal well more particularly, to one kind and divides
The high-temperature-reslow-viscosity low-viscosity high-shear water-in-oil drilling fluid of the special well type such as branch well.The present invention relates to the conjunction of the NiSe materials of different shape
Into, and material is furtherd investigate in DSSC to the application in electrode.
Background technology
DSSC (DSSCs), due to relatively low cost and higher photoelectric transformation efficiency (PCE)
It is widely studied.Past 20 years, in the research of efficiency, repeatability and stability, DSSCs achieved huge progress.
Generally, DSSCs is the TiO by being adsorbed with dyestuff2Light anode, to electrode (CE) and I3 -/I–Oxidation-reduction pair is constituted.Important
It is that the optimization of all battery components is all necessary for DSSCs superperformance.CE is mono- key components of DSSCs,
Oxidation-reduction pair regeneration and (2) are made to collect electronics and by electric transmission in electrolyte from external circuit with (1) catalyst
Oxidation state component.CE materials should possess high catalytic activity and the big advantage of electric conductivity two.Generally, Pt is deposited on FTO electro-conductive glass work
CE, Pt are electron collector as catalyst and FTO.Pt has proven to an outstanding CE catalyst, because its height is urged
Change the standard that activity and stability have developed as CE catalyst fields.However, Pt metal prices are expensive, in nature belong to dilute
There is metal.Limited Pt supply, it is impossible to meet growing large-scale production and application.Meanwhile, Pt can not be effectively catalyzed such as cobalt
Complex, T2/T-And polyelectrolyte.Therefore, the non-Pt electrode catalytic materialses of high-performance are developed, while but also with high conductivity and excellent
Catalytic activity more, the DSSCs for making it possible to the non-Pt of industrialization is favored by widely studied person.
The content of the invention
Possesses high conductivity and the non-Pt electrodes of superior catalytic activity are urged it is an object of the present invention to provide a kind of
Change material and preparation method thereof.
To reach above-mentioned purpose, the present invention uses following technical proposals：
NiSe electrocatalysis materials, NiSe electrocatalysis materials are the hexagonal crystal shape of sheet, and interplanar distance is 2 θ angles are
There is stronger absworption peak at 35.8 °, 42.7 °, 45.3 °, 59.0 °, 61.9 °, 68.8 °, 69.1 °, 82.5 °, 83.1 °；It is gathered in
It is in cotton-shaped pattern together.
The preparation method of above-mentioned NiSe electrocatalysis materials, comprises the following steps：
(1) Se powder and Nickel dichloride hexahydrate are added to the water, ultrasound；
(2) hydrazine hydrate solution, stirring are added；
(3) solution obtained in step (2) is transferred in autoclave, reacted under conditions of temperature is 180 DEG C；
(4) distinguish obtained solid 3-4 times in washing step (3) successively with deionized water and absolute ethyl alcohol, obtain product；
4h is dried in vacuo, black solid is obtained.
The preparation method of above-mentioned NiSe electrocatalysis materials, in step (1)：The amount of the material of Se powder and Nickel dichloride hexahydrate
The ratio between be (1.1-1.6)：1.
The preparation method of above-mentioned NiSe electrocatalysis materials, in step (1)：Per the amount of water used in 1mol Nickel dichloride hexahydrates
For 30-40mL.
The preparation method of above-mentioned NiSe electrocatalysis materials, in step (1)：Ultrasonic time is 20-50min.
The preparation method of above-mentioned NiSe electrocatalysis materials, in step (2)：Per hydrazine hydrate used in 1mol Nickel dichloride hexahydrates
The amount of solution is 20-30mL.
The preparation method of above-mentioned NiSe electrocatalysis materials, in step (2)：The concentration of hydrazine hydrate solution is 85wt%.
The preparation method of above-mentioned NiSe electrocatalysis materials, in step (3)：Reaction time is 3-10 hours.
The purposes of NiSe electrocatalysis materials, above-mentioned NiSe electrocatalysis materials are for DSSC to electrode
In.
Beneficial effects of the present invention are as follows：
The NiSe electrocatalysis materials that the present invention is prepared are to catalysis reduction I3 -Show excellent electro catalytic activity.Will
They are used for DSSC (DSSCs) to obtaining preferable photoelectric transformation efficiency in electrode, reach as high as
8.10%；Compared with standard Pt is the DSSCs performances (PCE=7.82%) to electrode, excellent electro catalytic activity is shown.
Brief description of the drawings
The embodiment to the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 NiSe-1 and NiSe-2 XRD.
Fig. 2 (a)：Different-shape NiSe-1 (a) and NiSe-2 (b) TEM schemes；
Fig. 2 (b)：Different-shape NiSe-1 (a) and NiSe-2 (b) TEM schemes；
Fig. 3 NiSe-1 and NiSe-2 impedance curve, illustration are breadboardin figure；
Fig. 4 NiSe-1 and NiSe-2 cyclic voltammetry curve；
The J-V curves for the DSSCs that Fig. 5 NiSe-1 and NiSe-2 are assembled respectively.
Embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
NiSe-1 synthesis：(1) 0.111gSe powder (1.4mmol) and 0.238g Nickel dichloride hexahydrates (1.0mmol), are added
Into 36mL water, ultrasonic 30min；(2) add the 24mL hydrazine hydrate solutions that concentration is 85wt%, stir 30min；(3) will be above-mentioned molten
Liquid is transferred to 100mL autoclaves, 180 DEG C of reaction 5h；(4) solid 4 is washed with deionized water and absolute ethyl alcohol respectively successively
It is secondary, obtain product；4h is dried in vacuo, black solid is obtained.
Embodiment 2 (synthetic method contrast test)
NiSe-2 synthesis：(1) 0.199g Ni (Ac) is weighed2, it is added in the phenmethylol containing 40mL, with 0.111g
SeO2Mixing；(2) heated at 180 DEG C after 20h, be cooled to room temperature；(3) filter, wash solid 3-4 with water and ethanol respectively
Secondary, solid vacuum drying 4h obtains black solid.
Electrochemical impedance spectroscopy EIS is tested
Electrochemical AC impedance analysis is for characterizing because electric charge occurs migration and occurs between electrode and electrolyte interface
Electrode reaction, can be between more accurate, sensitive reaction electrode and electrolyte interface electric charge reach dynamics.Specifically
Principle is the Sine Current Modulation perturbation signal by applying small amplitude to experimental system, sound of the test sine wave to modulating frequency
Answer at (amplitude and phase angle), corresponding collection of illustrative plates is referred to as electrochemical impedance spectroscopy.Electrochemical impedance spectroscopy is a kind of frequency domain test method,
Frequency range corresponding to different response speed parts is different, and what HFS reflected is the response of speed, low frequency part
Reflection is slow response.The small Shimmer signal applied answers battery system not produce influence, and keeps voltage
With the linear relationship of electric current, so as to later data processing.
Cyclic voltammetry curve is tested
Cyclic voltammetry (CV) is to judge one of common tool of reversibility of electrode and electro catalytic activity.In experiment, we
It can be tested using any detected materials as working electrode in corresponding electrolyte system.Herein will be to electrode system
Into 1.0 × 1.0cm2Size, using three-electrode system, it, to electrode, is platinum electrode to electrode that working electrode, which is, and reference electrode is
Ag+/ Ag electrodes are simultaneously demarcated with ferrocene, and sweep speed is 50mV s-1.Supporting electrolyte solution is I3 -/I-Anhydrous second
Nitrile solution.Instrument is the CHI660D instruments that Shanghai Chen Hua company produces.
As a result with discussion：
Fig. 1 is the XRD of NiSe-1 and NiSe-2 powder samples.From XRD it can be seen that：NiSe-1 is at 2 θ angles
There is stronger absworption peak to correspond to respectively at 35.8 °, 42.7 °, 45.3 °, 59.0 °, 61.9 °, 68.8 °, 69.1 °, 82.5 °, 83.1 °
Be NiSe crystal (101), (102), (110), (103), (201), (202), (004), (203), (211) diffraction crystal face.
NiSe-2 XRD, it can be seen that 2 θ angles at 28.2 °, 32.8 °, 44.3 °, 49.8 °, 59.4 °, 60.0 °, 68.8 °, 70.3 °,
81.1 °, it is NiSe crystal (100) that 82.5 ° are corresponding respectively, (101), (102), (110), (103), (201), (202),
(004), (203), (211) diffraction crystal face.All diffraction maximums are coincide well with the quasi- collection of illustrative plates card PDF#65-9451 of standard scale
(find and Ni i.e. in spectrum library:Se=1:1 similar standard diagram), other impurity peaks are not observed, show synthesis
Sample purity it is fine.
To being characterized by TEM for the NiSe-1 and NiSe-2 of different-shape.Can clearly it be observed by Fig. 2 (a)
It is laminated structure to NiSe-1, flocks together such as cotton-wool.By Fig. 2 (b) be NiSe-2 TEM, observable its be graininess.
Both high-resolution TEM have clearly lattice fringe, show the NiSe-1 and NiSe-2 of two kinds of different-shapes of synthesis and have
Good crystal property.Sheet can be obtained through survey calculation and granular NiSe-1 and NiSe-2 interplanar distances are respectivelyWithTheir interplanar distance (d good with hexagonal crystal shape NeSi [101] crystal face101) coincide well
(XRD is tested).Simultaneously as can be seen that sheet NiSe-1 interplanar distance is smaller than graininess NiSe-2The above results show that in building-up process [101] crystal face is easier to be exposed, and also further demonstrate and have synthesized two
Plant different-shape hexagonal crystal system NiSe materials.
It is prepared to electrode pair I in order to further evaluate3 -Reduction reaction electro catalytic activity, we are using structure
The Symmetrical cells of " to electrode/electrolyte/to electrode " obtain the Nyquist impedance spectrums (EIS) to electrode, as a result as shown in Figure 1.
Go out equivalent circuit diagram to evaluate the performance parameter to electrode using Randles models fittings.Generally, Nyquist figures include two
Individual semicircle, the semicircle of high frequency region is the charge transfer resistance R to electrode/electrolyte interfacect.Low frequency range semicircle is inside electrolyte
I3 -/ I- electricity to energy this special diffusion resistance (ZN).In addition, energy Si Tetu starting points correspond to string in the intercept of high frequency region real axis (Z ')
Join resistance Rs.Correlated fitting data are shown in Table 1.As can be seen that NiSe-1 and NiSe-2 RctRespectively 1.1 Ω and 10.3 Ω, have
Data can be seen that the NiSe-1 of cotton-shaped pattern, its RctR than graininess NiSe-2ctSmall, this shows the NiSe-1 of cotton-shaped pattern
More avtive spots are provided and participate in catalytic reaction, the catalytic activity of material of the catalytic activity than graininess NiSe-2 is high very
It is many.
Cyclic voltammetric is a kind of important means of electro-chemical activity for evaluating electrode material and combination property.
This, we use three-electrode system i.e. drop coating to be to be to electrode, Ag/Ag+ for working electrode, Pt by the FTO to electrode material
Reference electrode, electrolyte is 10m MLiI, 1m M I2, 0.1M LiClO4.Measure cyclic voltammetry curve as shown in Figure 4.As schemed
Shown, material Ni Se-1 and NiSe-2 in the scanning range that current potential is -1.0~1.0V, can observe two groups to the CV of electrode
Typical redox peaks.The mechanism and pertinent literature of electrode reaction are reported according to DSSCs, in composite to electrode material
CV curves in, the first redox peaks be formula (1) course of reaction, the second redox peaks be formula (2) reaction
Journey.Because during DSSCs is to electrode catalyst, its major function is catalysis reduction I3 -.Therefore, the first redox peaks conduct
The emphasis of research.In addition, peak-to-peak away from E between first pair of redox peaksppIt is also to weigh electrode catalyst with peak position current density
The important parameter of ability, wherein EppValue is smaller, shows that the catalytic activity of electrode material is higher；Peak current is bigger, respective material
Catalytic performance is also better.NiSe-1 and NiSe-2 the first redox spike potential spacing Epp(0.28V) is than NiSe-2 to electrode
Epp(0.57V) greatly, this, which also indicates that NiSe-1 as electrocatalysis material, preferable catalytic activity.
I3 -+2e-=3I- (1)
3I2+2e-=2I3 - (2)
The parameter and electrochemical data of the impedance diagram of table 1 fitting.
The different DSSCs to electrode assembling of table 2 photovoltaic parameter.
Fig. 5 compares the different DSSCs to electrode assembling J-V curves, and the photovoltaic performance parameter of battery is shown in Table 2.With
NiSe-1 is 8.10% (V to the DSSC of electrode assembling PCEoc=736mV, Jsc=15.17mA cm-2, FF=0.73).With
NiSe-2 is to the DSSCs of electrode assembling, (Voc=731mV, Jsc=14.86mA cm-2, FF=0.72, PCE=7.44%).Phase
For NiSe-2, using NiSe-1 as the DSSCs to electrode, its energy conversion efficiency improves 8.8%.As a result have with NiSe-1
Preferable electro catalytic activity is consistent.Moreover, compared with standard Pt is the DSSCs performances (PCE=7.82%) to electrode, base
It is the good photoelectricity effect also obtained to electrode DSSCs in NiSe-1.The above results show, the NiSe-1 nanometers of sheet-like morphology
Material is expected to applied to DSSCs in electrode.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (9)
1.NiSe electrocatalysis materials, it is characterised in that NiSe electrocatalysis materials are the hexagonal crystal shape of sheet, interplanar distance is2 θ angles are to have stronger at 35.8 °, 42.7 °, 45.3 °, 59.0 °, 61.9 °, 68.8 °, 69.1 °, 82.5 °, 83.1 °
Absworption peak；Flock together in cotton-shaped pattern.
The preparation method of 2.NiSe electrocatalysis materials, it is characterised in that comprise the following steps：
(1) Se powder and Nickel dichloride hexahydrate are added to the water, ultrasound；
(2) hydrazine hydrate solution, stirring are added；
(3) solution obtained in step (2) is transferred in autoclave, reacted under conditions of temperature is 180 DEG C；
(4) distinguish obtained solid 3-4 times in washing step (3) successively with deionized water and absolute ethyl alcohol, obtain product；Vacuum
4h is dried, black solid is obtained.
3. the preparation method of NiSe electrocatalysis materials according to claim 1, it is characterised in that in step (1)：Se powder
It is (1.1-1.6) with the ratio between the amount of material of Nickel dichloride hexahydrate：1.
4. the preparation method of NiSe electrocatalysis materials according to claim 3, it is characterised in that in step (1)：Often
The amount of water used in 1mol Nickel dichloride hexahydrates is 30-40mL.
5. the preparation method of NiSe electrocatalysis materials according to claim 4, it is characterised in that in step (1)：Ultrasound
Time is 20-50min.
6. the preparation method of NiSe electrocatalysis materials according to claim 1, it is characterised in that in step (2)：Often
The amount of hydrazine hydrate solution used in 1mol Nickel dichloride hexahydrates is 20-30mL.
7. the preparation method of NiSe electrocatalysis materials according to claim 6, it is characterised in that in step (2)：Hydration
The concentration of hydrazine solution is 85wt%.
8. the preparation method of NiSe electrocatalysis materials according to claim 1, it is characterised in that in step (3)：Reaction
Time is 3-10 hours.
The purposes of 9.NiSe electrocatalysis materials, it is characterised in that it is quick that the NiSe electrocatalysis materials in claim 1-9 are used for dyestuff
Change solar cell in electrode.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108376612A (en) * | 2018-01-24 | 2018-08-07 | 复旦大学 | Preparation method of the used by dye sensitization solar battery graphene/nickelous selenide to electrode |
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| CN102610392A (en) * | 2012-03-21 | 2012-07-25 | 复旦大学 | Metal selenide counter-electrode for dye-sensitized solar cell and preparation method of metal selenide counter-electrode |
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2017
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| CN102583273A (en) * | 2012-02-13 | 2012-07-18 | 安徽大学 | Method for preparing nano nickel selenide with octahedral structure |
| CN102610392A (en) * | 2012-03-21 | 2012-07-25 | 复旦大学 | Metal selenide counter-electrode for dye-sensitized solar cell and preparation method of metal selenide counter-electrode |
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| CN108376612A (en) * | 2018-01-24 | 2018-08-07 | 复旦大学 | Preparation method of the used by dye sensitization solar battery graphene/nickelous selenide to electrode |
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Application publication date: 20170721 |