CN106206042A - A kind of DSSC NiSe preparation method to electrode - Google Patents
A kind of DSSC NiSe preparation method to electrode Download PDFInfo
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- CN106206042A CN106206042A CN201610653669.XA CN201610653669A CN106206042A CN 106206042 A CN106206042 A CN 106206042A CN 201610653669 A CN201610653669 A CN 201610653669A CN 106206042 A CN106206042 A CN 106206042A
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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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- 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 invention discloses a kind of DSSC NiSe preparation method to electrode, its step is as follows: added in deionized water by 0.01mol ~ 1.03mol hydrazine hydrate, adds 0.05mmol ~ 0.6mol selenium powder, and stirring, to being completely dissolved, forms mixed solution；The nickel sheet cleaned up is put in water heating kettle, pours mixed solution into；100 DEG C ~ 200 DEG C, carry out hydro-thermal reaction under the conditions of 2 ~ 24h, naturally cool to room temperature, take out sample, wash and be dried and can be used as electrode is used.NiSe disclosed by the invention is simple to the preparation technology of electrode, cheap, and manufacturing cycle is short, easy to operate, can carry out the preparation of rapid, high volume；Meanwhile, preparation good to electrode conductivity, fill factor, curve factor is high, catalysis activity good, have excellence photoelectric transformation efficiency.
Description
Technical field
The invention belongs to nano material preparation technology and energy field, relate to a kind of DSSC to electrode
The preparation method of material.
Background technology
Along with the high speed development of society, traditional energy drastically consumes, and the exhaustion the most increasingly of its reserves, energy problem seems always
Being all potential crisis, thing followed environmental problem is the most increasingly concerned, the most actively seek and develop pollution-free, can be again
Raw new forms of energy are extremely the most urgent.People in the exploration of regenerative resource and research, solar energy is with its rich reserves, cleaning
The advantage such as pollution-free, reliable is considered the preferable energy of the mankind.Present stage is concentrated mainly on photo-thermal to the utilization of solar energy
Conversion, Photochemical convertion and opto-electronic conversion, and the principal mode of opto-electronic conversion is solaode, it is solving energy crisis side
Face can preferably play a role.
As a member of solaode family, DSSC is simple due to its low cost, preparation technology
Also get most of the attention with photoelectric transformation efficiency advantages of higher.DSSC mainly by appendix the light anode of dyestuff,
Electrolyte and to three, electrode part composition.To electrode as reducing catalyst, except collecting and transport the electronics of external circuit, also
There is I in catalytic electrolysis matter3 -It is reduced to I-Deng effect, generally at transparent conductive glass surface plating last layer platinum as dye sensitization
Solaode is to electrode, but Pt belongs to noble metal, and the price of its costliness adds the cost of battery, is not appropriate for as dyestuff
Sensitization solar battery industrialization preferable to electrode material.
Transition metal selenides is owing to having much special character, and wide material sources, cost is the cheapest, thus quilt
It is widely used in DSSC to electrode material.Wherein, the one step hydro thermal method that the present invention provides synthesizes NiSe pair
Electrode, preparation technology is simple, cheap, and material source enriches, prepared good to electrode conductivity, electro catalytic activity good, fill
The factor is high, and good stability can promote the photoelectric transformation efficiency of DSSC effectively.
Summary of the invention
The invention aims to solve that existing DSSC is expensive to electrode material, be not suitable for
The present situation of large-scale application, it is provided that a kind of DSSC NiSe preparation method to electrode one step hydro-thermal.
The present invention is achieved by the following technical solutions:
(1) preparation mixed solution: by 0.01mol ~ 1.03mol hydrazine hydrate (or 0.01mmol ~ 0.5mol NaBH4、KBH4Deng)
Adding in deionized water, add 0.05mmol ~ 0.6mol selenium powder, stirring, to being completely dissolved, forms mixed solution.
(2) nickel sheet cleaned up is put in 50mL water heating kettle, pour mixed solution into, under the conditions of 100 DEG C ~ 200 DEG C
Carry out hydro-thermal reaction 2 ~ 24h, naturally cool to room temperature, take out sample, wash and be drying to obtain electrode.
The invention provides a kind of DSSC NiSe step hydrothermal preparing process to electrode.The method
Preparation technology is simple, cheap, and material source enriches, prepared good to electrode conductivity, electro catalytic activity good, fill factor, curve factor
Height, good stability, can effectively promote the photoelectric transformation efficiency of DSSC.
Accompanying drawing explanation
The amount of the material of Fig. 1 (a) reactant is respectively 1.6mmol NaBH4, 2.5mmol selenium powder 140 DEG C of conditions next
The step NiSe prepared by hydro-thermal reaction 12h SEM photograph under 1 μm multiple；B the amount of the material of () reactant is respectively
0.082mol hydrazine hydrate, 2.5mmol selenium powder at the NiSe prepared by 140 DEG C of next step hydro-thermal reactions 12h of condition under 1 μm multiple
SEM photograph；
Fig. 2 Ca is to add the hydrazine hydrate of amount of different material and 2.5mmol selenium powder 140 DEG C of next step hydro-thermal reactions 12h of condition
The prepared DSSCs that electrode is assembled current density voltage curve under standard analog sunlight；Cb is for adding
The NaBH of the amount of different material4And 2.5mmol selenium powder prepared by 140 DEG C of next step hydro-thermal reactions 12h of condition to electrode institute
The DSSCs assembled current density voltage curve under standard analog sunlight；Cc is the selenium of the amount adding different material
Powder and 1.6mmol NaBH4At the DSSCs that electrode is assembled prepared by 140 DEG C of next step hydro-thermal reactions 12h of condition at mark
Quasi-mode intends the current density voltage curve under sunlight；
The amount of the material of Fig. 3 reactant is respectively 1.6mmol NaBH4(or 0.082mol hydrazine hydrate), 2.5mmol selenium powder is not
The DSSCs being assembled electrode prepared by synthermal or next step hydro-thermal reaction of time conditions is in standard analog sunlight
Under current density voltage curve.
Detailed description of the invention
Below in conjunction with instantiation, technical scheme is described in further detail, but the protection model of the present invention
Enclose and be not limited thereto.
Embodiment 1 reduction system is NaBH4Time one step hydro thermal method prepared by electrode
By 0.3mol NaBH4Adding in deionized water, add 2.5mmol selenium powder, stirring, to being completely dissolved, forms mixing molten
Liquid；The nickel sheet cleaned up is put in 50mL water heating kettle, pours mixed solution into, under the conditions of 140 DEG C, carry out hydro-thermal reaction
12h, naturally cools to room temperature, takes out sample, washs and be drying to obtain electrode.
(1) prepared sample carries out surface scan Electronic Speculum (SEM) characterize, as it is shown in figure 1, wherein (a) is for adding
1.6mmol NaBH4Time prepared NiSe electrode is had nanowire array structure, the nanostructured of this uniqueness has relatively
Many avtive spots, and the diffusion of beneficially electrolyte, thus the activity of the catalysis to electrode can be significantly improved.
(2) using sample as to electrode, it is assembled into battery, carries out device performance test.Electrolyte proportioning is: 0.1M 1-
Propy-3-methylimidazolium iodide (1-propyl group-3-Methylimidazole. iodine), 0.05M LiI, 0.1M GNCS,
0.03M I2, 0.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent is the mixing of propene carbonate and acetonitrile
Solution (volume ratio is 1:1).(the synthetic method reference of light anode: S. Ito, T. Murakami, P. Comte, P.
Liska, C. Grätzel, M. Nazeeruddin, M. Grätzel, Thin Solid Films, 516 (2008)
4613-4619.).
Simulated solar radiant xenon lamp (Oriel 91192, USA, irradiation intensity 100W/cm is used during test2), electrification
Learning the instruments such as work station, dark slide light-permeable is shown up and is amassed as 0.25cm2.Test result is as shown in Cb in Fig. 2, wherein: Cb1For adding
Enter 1mmol NaBH4Time prepare to electrode, Cb2For adding 1.6mmol NaBH4Time prepare to electrode.Cb1Corresponding photovoltaic
Parameter is: Voc=0.67V, Jsc=14.2mA cm-2, FF=0.67, PCE=6.35%.Cb2Corresponding photovoltaic parameter is: Voc=
0.66V, Jsc=15.64mA cm-2, FF=0.67, PCE=6.89%, it is better than Pt electrode (Voc=0.61V, Jsc=16.61mA
cm-2, FF=0.63, PCE=6.34%), absolutely prove that the sample prepared by hydro-thermal method has higher fill factor, curve factor and electricity is urged
Change activity, thus obtain higher photoelectric transformation efficiency.
When embodiment 2 reduction system is hydrazine hydrate prepared by one step hydro thermal method to electrode
Being added in deionized water by 1.03mol hydrazine hydrate, add 2.5mmol selenium powder, stirring, to being completely dissolved, forms mixing molten
Liquid；The nickel sheet cleaned up is put in 50mL water heating kettle, pours mixed solution into, under the conditions of 140 DEG C, carry out hydro-thermal reaction
12h, naturally cools to room temperature, takes out sample, washs and be drying to obtain electrode.
(1) prepared sample carries out surface scan Electronic Speculum (SEM) characterize, as it is shown in figure 1, wherein (b) is for adding
NiSe prepared during 0.082mol hydrazine hydrate has nano rod array structure to electrode, and the nanostructured of this uniqueness has
More avtive spot, and the diffusion of beneficially electrolyte, thus the activity of the catalysis to electrode can be significantly improved.
(2) using sample as to electrode, it is assembled into battery, carries out device performance test.Electrolyte proportioning is: 0.1M 1-
Propy-3-methylimidazolium iodide (1-propyl group-3-Methylimidazole. iodine), 0.05M LiI, 0.1M GNCS,
0.03M I2, 0.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent is the mixing of propene carbonate and acetonitrile
Solution (volume ratio is 1:1).(the synthetic method reference of light anode: S. Ito, T. Murakami, P. Comte, P.
Liska, C. Grätzel, M. Nazeeruddin, M. Grätzel, Thin Solid Films, 516 (2008)
4613-4619.).
Simulated solar radiant xenon lamp (Oriel 91192, USA, irradiation intensity 100W/cm is used during test2), electrification
Learning the instruments such as work station, dark slide light-permeable is shown up and is amassed as 0.25cm2.Test result is as shown in Ca in Fig. 2, wherein: Ca1For adding
Prepare when entering 0.041mol hydrazine hydrate to electrode, Ca2For add 0.082mol hydrazine hydrate time prepare to electrode.Ca1Accordingly
Photovoltaic parameter be: Voc=0.68V, Jsc=14.25mA cm-2, FF=0.66, PCE=6.36%.Ca2Corresponding photovoltaic parameter
For: Voc=0.66V, Jsc=16.52mA cm-2, FF=0.65, PCE=7.10%, it is better than Pt electrode (Voc=0.61V, Jsc=
16.61mA·cm-2, FF=0.63, PCE=6.34%), absolutely proved the sample prepared by hydro-thermal method have higher filling because of
Son and electro catalytic activity, thus obtain higher photoelectric transformation efficiency.
The selenium powder of the amount of embodiment 3 different material participate in prepared by reaction to electrode
By 1.6mmol NaBH4Add in deionized water, add 0.05mmol ~ 0.6mol selenium powder, stir to being completely dissolved,
Form mixed solution；The nickel sheet cleaned up is put in 50mL water heating kettle, pours mixed solution into, carry out under the conditions of 140 DEG C
Hydro-thermal reaction 12h, naturally cools to room temperature, takes out sample, washs and be drying to obtain electrode.
Using sample as to electrode, it is assembled into battery, carries out device performance test.Electrolyte proportioning is: 0.1M 1-
Propy-3-methylimidazolium iodide (1-propyl group-3-Methylimidazole. iodine), 0.05M LiI, 0.1M GNCS,
0.03M I2, 0.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent is the mixing of propene carbonate and acetonitrile
Solution (volume ratio is 1:1).(the synthetic method reference of light anode: S. Ito, T. Murakami, P. Comte, P.
Liska, C. Grätzel, M. Nazeeruddin, M. Grätzel, Thin Solid Films, 516 (2008)
4613-4619.).
Simulated solar radiant xenon lamp (Oriel 91192, USA, irradiation intensity 100W/cm is used during test2), electrification
Learning the instruments such as work station, dark slide light-permeable is shown up and is amassed as 0.25cm2.Test result is as shown in Cc in Fig. 2, wherein: Cc1For adding
Prepare when entering 0.75mmol selenium powder to electrode, Cc2For add 2.5mmol selenium powder time prepare to electrode.Cc1Corresponding photovoltaic
Parameter is: Voc=0.64V, Jsc=14.04mA cm-2, FF=0.68, PCE=6.11%.Cc2Corresponding photovoltaic parameter is: Voc=
0.66V, Jsc=15.64mA cm-2, FF=0.67, PCE=6.89%, it is better than Pt electrode (Voc=0.61V, Jsc=16.61mA
cm-2, FF=0.63, PCE=6.34%), absolutely prove that the sample prepared by hydro-thermal method has higher fill factor, curve factor and electricity is urged
Change activity, thus obtain higher photoelectric transformation efficiency.
At a temperature of embodiment 4 differential responses prepared by hydro-thermal to electrode
Being added in deionized water by 0.082mol hydrazine hydrate, add 2.5mmol selenium powder, stirring, to being completely dissolved, forms mixing
Solution；The nickel sheet cleaned up is put in 50mL water heating kettle, pours mixed solution into, under the conditions of 100 DEG C ~ 200 DEG C, carry out water
Thermal response 12h, naturally cools to room temperature, takes out sample, washs and be drying to obtain electrode.
Using sample as to electrode, it is assembled into battery, carries out device performance test.Electrolyte proportioning is: 0.1M 1-
Propy-3-methylimidazolium iodide (1-propyl group-3-Methylimidazole. iodine), 0.05M LiI, 0.1M GNCS,
0.03M I2, 0.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent is the mixing of propene carbonate and acetonitrile
Solution (volume ratio is 1:1).(the synthetic method reference of light anode: S. Ito, T. Murakami, P. Comte, P.
Liska, C. Grätzel, M. Nazeeruddin, M. Grätzel, Thin Solid Films, 516 (2008)
4613-4619.).
Simulated solar radiant xenon lamp (Oriel 91192, USA, irradiation intensity 100W/cm is used during test2), electrification
Learning the instruments such as work station, dark slide light-permeable is shown up and is amassed as 0.25cm2.Test result is as it is shown on figure 3, wherein: reaction temperature is
Under the conditions of 120 DEG C, the photovoltaic parameter that electrode is corresponding is by gained: Voc=0.65V, Jsc=13.7mA cm-2, FF=0.66, PCE=
5.86%.Under the conditions of reaction temperature is 140 DEG C, the photovoltaic parameter that electrode is corresponding is by gained: Voc=0.63V, Jsc=
15.58mA·cm-2, FF=0.69, PCE=6.75%, it is better than Pt electrode (Voc=0.61V, Jsc=16.61mA cm-2, FF=
0.63, PCE=6.34%).Under the conditions of reaction temperature is 160 DEG C, the photovoltaic parameter that electrode is corresponding is by gained: Voc=0.65V,
Jsc=15.02mA·cm-2, FF=0.68, PCE=6.63%, it is better than Pt electrode (Voc=0.61V, Jsc=16.61mA cm-2, FF
=0.63, PCE=6.34%).Absolutely prove that the sample prepared by hydro-thermal method has higher fill factor, curve factor and electro catalytic activity,
Thus obtain higher photoelectric transformation efficiency.
Under the embodiment 5 differential responses time prepared by hydro-thermal to electrode
By 1.6mmol NaBH4Adding in deionized water, add 2.5mmol selenium powder, stirring, to being completely dissolved, forms mixing molten
Liquid；The nickel sheet cleaned up is put in 50mL water heating kettle, pours mixed solution into, carry out under the conditions of 140 DEG C hydro-thermal reaction 2 ~
24h, naturally cools to room temperature, takes out sample, washs and be drying to obtain electrode.
Using sample as to electrode, it is assembled into battery, carries out device performance test.Electrolyte proportioning is: 0.1M 1-
Propy-3-methylimidazolium iodide (1-propyl group-3-Methylimidazole. iodine), 0.05M LiI, 0.1M GNCS,
0.03M I2, 0.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent is the mixing of propene carbonate and acetonitrile
Solution (volume ratio is 1:1).(the synthetic method reference of light anode: S. Ito, T. Murakami, P. Comte, P.
Liska, C. Grätzel, M. Nazeeruddin, M. Grätzel, Thin Solid Films, 516 (2008)
4613-4619.).
Simulated solar radiant xenon lamp (Oriel 91192, USA, irradiation intensity 100W/cm is used during test2), electrification
Learning the instruments such as work station, dark slide light-permeable is shown up and is amassed as 0.25cm2.Test result is as it is shown on figure 3, wherein: the response time is
Under the conditions of 6h, the photovoltaic parameter that electrode is corresponding is by gained: Voc=0.62V, Jsc=15.64mA cm-2, FF=0.68, PCE=
6.55%, it is better than Pt electrode (Voc=0.61V, Jsc=16.61mA cm-2, FF=0.63, PCE=6.34%).Response time is
Under the conditions of 12h, the photovoltaic parameter that electrode is corresponding is by gained: Voc=0.65V, Jsc=15.56mA cm-2, FF=0.67, PCE=
6.80%, it is better than Pt electrode (Voc=0.61V, Jsc=16.61mA cm-2, FF=0.63, PCE=6.34%).Response time is
Under the conditions of 18h, the photovoltaic parameter that electrode is corresponding is by gained: Voc=0.65V, Jsc=15.02mA cm-2, FF=0.68, PCE=
6.63%, it is better than Pt electrode (Voc=0.61V, Jsc=16.61mA cm-2, FF=0.63, PCE=6.34%).Absolutely prove water
Sample prepared by full-boiled process has higher fill factor, curve factor and electro catalytic activity, thus obtains higher photoelectric transformation efficiency.
Claims (2)
1. the DSSC NiSe preparation method to electrode, it is characterised in that described method step is as follows:
Step one: added in deionized water by reducing agent hydrazine hydrate, add selenium powder, until being completely dissolved, forms mixed solution；
Step 2: nickel sheet cleaned up, puts in water heating kettle as base material with reaction primitive, and the mixing pouring step one into is molten
Liquid, seals；
Step 3: hydro-thermal reaction 2 ~ 24h under conditions of 100 DEG C ~ 200 DEG C, naturally cools to room temperature after having reacted, take out examination
It is cleaned multiple times with deionized water and ethanol after sample, is dried, is DSSC NiSe to electrode.
The DSSC NiSe the most according to claim 1 preparation method to electrode, it is characterised in that
Described reducing agent hydrazine hydrate can also use NaBH4Or KBH4Substitute, when reducing agent is hydrazine hydrate, hydrazine hydrate in mixed solution
The amount of material be 0.01mol ~ 1.03mol；When reducing agent is NaBH4Or KBH4Time, NaBH in mixed solution4Or KBH4Thing
The amount of matter is 0.01mmol ~ 0.5mol；In mixed solution, the amount of the material of selenium powder is 0.05mmol ~ 0.6mol.
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| CN107275096A (en) * | 2017-07-20 | 2017-10-20 | 石河子大学 | Copper selenium sulphur to electrode, preparation method, using and quantum dot sensitized solar cell |
| 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 |
| CN108493297A (en) * | 2018-03-23 | 2018-09-04 | 福州大学 | A kind of preparation method of three-dimensional hollow selenium nanometer nickel sulfide frame catalyst |
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