CN106241852A - A kind of Pr (OH)3the preparation method of monodimension nano stick - Google Patents
A kind of Pr (OH)3the preparation method of monodimension nano stick Download PDFInfo
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- CN106241852A CN106241852A CN201610587957.XA CN201610587957A CN106241852A CN 106241852 A CN106241852 A CN 106241852A CN 201610587957 A CN201610587957 A CN 201610587957A CN 106241852 A CN106241852 A CN 106241852A
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- praseodymium
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 27
- 150000001213 Praseodymium Chemical class 0.000 claims abstract description 15
- 238000009713 electroplating Methods 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 10
- 238000004146 energy storage Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical group [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 claims description 3
- PRORZGWHZXZQMV-UHFFFAOYSA-N azane;nitric acid Chemical group N.O[N+]([O-])=O PRORZGWHZXZQMV-UHFFFAOYSA-N 0.000 claims 1
- ZLGIGTLMMBTXIY-UHFFFAOYSA-K praseodymium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Pr+3] ZLGIGTLMMBTXIY-UHFFFAOYSA-K 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- 238000011161 development Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical group OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 3
- 229910052777 Praseodymium Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- BOJUHNOLOKDHBE-UHFFFAOYSA-N praseodymium;hydrate Chemical compound O.[Pr] BOJUHNOLOKDHBE-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- 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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention provides a kind of Pr (OH)3The preparation method of monodimension nano stick.Described preparation method is configuration precursor solution, generates Pr (OH) by step constant current galvanoplastic at working electrode surface3Monodimension nano stick；Described precursor solution is the mixed aqueous solution of praseodymium salt and ammonium salt, and in described precursor solution, the concentration of praseodymium salt is (1 ~ 8) g/L；The mixing ratio of described praseodymium salt and ammonium salt is (1 ~ 7): 1.Described electroplating temperature is 60 ~ 80 DEG C, and electroplating current is 1.5 2 mA.Described electroplating time is 1 ~ 3h.Preparation method energy consumption of the present invention is low, simple to operate, it is easy to accomplish scale, the Pr (OH) prepared31-dimention nano bar material, by high-specific surface area and the electrochemical capacitance performance of Praseodymium trihydroxide monodimension nano stick, it is possible to effectively store the energy, provide good material for current energy storage problem, possess great application prospect.
Description
Technical field
The present invention relates to energy storage field of material technology, more particularly, to a kind of Pr (OH)3The system of monodimension nano stick
Preparation Method.
Background technology
As the important substance basis of human society and economic development, energy problem always annoyings a weight of society
Want problem.Along with explosive growth and the fast development of society of population, the mankind are the most growing to the various demands of the energy.But
Being as the non-renewable and excessive exploitation of traditional fossil energy, the existing energy resource structure based on traditional fossil energy is bright
Show and can not meet the Future Society various demands to the energy for a long time.It addition, along with the exploitation of fossil energy, greenhouse effect day
Benefit is serious, and ecological environment goes from bad to worse, and pure and reproducible green energy resource has become as focus of concern.The such as sun
The a series of new green powers such as energy, wind energy, geothermal energy, ocean energy often also exist the unbalanced problem of Area distribution, are subject to
It is limited to natural conditions, it usually needs be translated into electric energy just convenient use.Owing to the demand in area is not mated, generally need
Want a power storage system by unnecessary energy storage, be allowed to again when demand discharge and be utilized again.So
Realizing the deep development of new forms of energy and efficiently utilize, the development of new and effective, stable electrical energy storage device is crucial.
Ultracapacitor, is again electrochemical capacitor, is novel between battery and traditional capacitor of a kind of performance
Energy storing device, has the plurality of advantages such as power density high, charge/discharge rates fast, length in service life, environmental friendliness.With tradition
Capacitor compare, ultracapacitor has higher energy density；And compared with battery, ultracapacitor then has higher
Power density and cyclical stability.Additionally, ultracapacitor can also be used in combination with the battery such as fuel cell, Ni-MH battery,
Not only can meet the electric automobile high power requirements when starting, accelerating and climb, and again can be fast when braking automobile
The big electric current that speed storage electromotor produces, thus effectively reduce the high current charge-discharge destruction to battery, reach to extend battery
Life-span effect.Therefore, ultracapacitor be widely used in electric automobile, computer stand-by power supply, emergency lighting,
The fields such as signal monitoring.In view of it is widely applied prospect, the developed country such as the most American-European, Japanese, Russian is all to super electricity
Container gives the attention of height, and puts into great dynamics and research and develop.China also increases the research and development power of ultracapacitor
Degree, and ultracapacitor is listed in " national medium-term and long-term scientific and technological development outline " (2005-2020).Therefore, deeply open
The research of exhibition ultracapacitor has important application value.
The Pr (OH) found at present3Material, is used for the aspects such as chemical industry, oil, electronic device, permanent magnet material more,
Report in terms of electrochemical capacitance seldom occurs.Praseodymium (Pr) belongs to periodic system III B race, rare earth element, lanthanide series.It is as large usage quantity
Rare earth element, be to be utilized with the form of mischmetal greatly, such as purification alterant, the change of metal material
Work catalyst, agricultural rare-earth etc..Additionally, rare earth permanent-magnetic material is also a big hot topic application of praseodymium.Its oxide and hydrogen-oxygen
Compound is gathered around in fields such as magnetic material, catalysis material, hydrogen storage material, optics and is had broad application prospects.As a wiener
Rice structural material, Pr (OH)3Nanometer rods have other excellent properties, as huge specific surface area, electric transmission path shorten,
Electric conductivity promotes.Therefore Pr (OH) in the present invention3The high-specific surface area of material, low electric transmission path is integrated, is effectively increased
Avtive spot, improves the electric conductivity of electrode, further increases the electrochemical capacitance performance of electrode.Additionally, current nano material
Production in enormous quantities still limit the development of nano material.Method designed by the present invention is that it further applies energy storage
Solid theory and practice basis has been laid in field.
Summary of the invention
It is an object of the invention to according to the deficiencies in the prior art, it is provided that a kind of Pr (OH)3The preparation of monodimension nano stick
Method.
Preparation method of the present invention can overcome electrochemical capacitance negative material large-scale production in prior art only to limit to
Problem in carbon-based material.The Pr (OH) that the present invention prepares3Monodimension nano stick as electrochemical capacitance negative material, and can possess
Excellent capacitive property.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
The invention provides a kind of Pr (OH)3The preparation method of monodimension nano stick, described preparation method is configuration precursor solution,
Pr (OH) is generated at working electrode surface by step constant current galvanoplastic3Monodimension nano stick；Described precursor solution is praseodymium salt
With the mixed aqueous solution of ammonium salt, in described precursor solution, the concentration of praseodymium salt is (1 ~ 8) g/L；Described praseodymium salt and the mixing of ammonium salt
Than being (1 ~ 7): 1；Described electroplating temperature is 60 ~ 80 DEG C, and electroplating current is 1.5-2 mA；Described electroplating time is 1 ~ 3h.
Preferably, in described precursor solution, the concentration of praseodymium salt is 4.5g/L；The mixing ratio of described praseodymium salt and ammonium salt is 3:
1。
Preferably, described electroplating temperature is 70 DEG C, and electroplating current is 2 mA；Described electroplating time is 2h.
Preferably, described praseodymium salt is praseodymium nitrate, and described ammonium salt is ammonium nitrate.
Preferably, described working electrode is conduction carbon cloth, conductive metal material or the FTO glass that conducts electricity.
Preferably, described working electrode is titanium sheet, and platinum electrode is to electrode.
The present invention uses working electrode as carrier, Pr (OH)3Monodimension nano stick is formed on this carrier, and this carrier is permissible
It is conduction carbon cloth or the titanium sheet, copper sheet, conduction FTO glass etc. of multiple conventional conductive carrier, such as business.
Electrode material prepared by the present invention, can be used as super capacitor material, solves existing Pr (OH)3Material compares table
The problem that the low avtive spot caused of area is few.
In the inventive solutions, by setting component and the ratio thereof of suitable precursor solution, to hydroxide
The Morphological control of praseodymium nano material so that it is controllable growth；By setting suitable response time and temperature, it is thus achieved that suitable one
The size of dimension praseodymium hydroxide nanometer rod；By setting suitable loading current so that Praseodymium trihydroxide can on carrier surface uniformly
Growth.
The present invention uses step constant current galvanoplastic to prepare Pr (OH)3Material, overcomes employing hydro-thermal method in prior art
Etc. directly can not generating the defect of target product on carrier, meanwhile, the material that hydro-thermal method generates due to do not have carrier as
Support, self specific surface area is smaller, causes its avtive spot relatively low.
Compared with prior art, the method have the advantages that
The present invention directly will synthesize the Pr (OH) with high-specific surface area on carrier3Monodimension nano stick, thus improve electricity
The specific surface area of pole material, significantly increases the avtive spot of electrode surface, thus increase effectively the capacitive character of electrode material
Energy.Further, since the character that monodimension nanometer material is exclusive, electric transmission path shortens, and is more beneficial for the expression of capacitive property.
The present invention is by controlling preparation condition simultaneously, has regulated and controled Pr (OH)3The growth of nano material, it is thus achieved that capacitive property carries further
The target product risen.
Accompanying drawing explanation
Fig. 1: (a) is Pr (OH) in embodiment 13Low range scanning electron microscope (SEM) picture of nanometer rods, (b) is embodiment 1
Middle Pr (OH)3High magnification scanning electron microscope (SEM) picture of nanometer rods；
Fig. 2: (a) is Pr (OH) in embodiment 13X-ray diffraction (XRD) spectrogram of nanometer rods, (b) is Pr in embodiment 1
(OH)3Nanometer rods cyclic voltammetry curve under 100 mV/s.
Detailed description of the invention
Further illustrate the present invention below in conjunction with Figure of description and specific embodiment, but embodiment is not to the present invention
Limit in any form.Unless stated otherwise, the present invention uses reagent, method and apparatus are the examination of the art routine
Agent, method and apparatus.
Unless stated otherwise, agents useful for same of the present invention and material are commercial.
Embodiment 1:
Pr(OH)3Nanometer rods in titanium sheet be synthesized by galvanostatic method realize.Before galvanostatic method current load, titanium sheet
(1.5 cm × 3 cm) is going from water, ethanol, acetone, deionized water ultrasonic cleaning 10 minutes respectively, then with compression successively
Air blow drying is standby.The titanium sheet cleaned up is immersed the forerunner's aqueous solution mixed equipped with 20 ml praseodymium nitrates and ammonium nitrate
Two electrode systems in, the most corresponding six nitric hydrate praseodymium 90 mg, corresponding ammonium nitrate 30 mg.Using titanium sheet as working electrode,
With platinum electrode for electrode, two electrode systems are placed in the oil bath pan of 70 DEG C.After system temperature is stable, system is applied
The loading current of negative 2.0 mA, and keep reacting 2 h.Titanium sheet is taken out after terminating by reaction, and gained sample spends from water the most clear
Wash three times, 60 DEG C of drying.
Performance test: the Pr (OH) to preparation3Nanometer rods has carried out the test of Flied emission scanning electron microscopy Electronic Speculum.Result is such as
Shown in Fig. 1, scanning electron microscope diagram shows one-dimensional Pr (OH)3Nanometer rods can be homogeneous, regular be grown in titanium sheet.From
Fig. 1 a, b medium scale is it can be seen that Pr (OH)3The length of nanometer rods is in 1.5-2.0 μm, and diameter is about 130 nm.Fig. 2 a adopts
With X-ray powder diffraction test, it is higher, for Pr (OH) that test shows to test gained sample crystallization degree3Material；Fig. 2 b uses
Its electrochemical capacitance performance is studied in cyclic voltammetry test in electrochemical method, by cyclic voltammetry curve it can be seen that its
Curve shows extraordinary reversibility, and the figure that curve surrounds is approximate rectangular.By calculating, this sample specific area electric capacity
Value is 0.16mF/cm2, this is reported first Pr (OH) in the middle of existing document3The capacitance characteristic of material.Thus judge, this one
Dimension Pr (OH)3Nano-bar material shows certain electrochemical capacitance performance, and the application in terms of energy storage has the biggest prospect.
Embodiment 2 ~ 5
Scheme based on embodiment 1, by regulating and controlling different reaction conditions, affects Pr (OH)3Growth, its relation such as table 1 institute
Show.
Wherein, embodiment 2 and 3 explanation temperature factor is relatively big on material preparation impact, and embodiment 4 illustrates precursor solution
Material preparation has been affected by mixed proportion factor, and embodiment 5 illustrates that response time factor can restrict Material growth length.Described
Embodiment 2 ~ 5 all can prepare Pr (OH)3Material, but pattern is poor comparatively speaking, and specific surface area is less, reactivity site
Few, electrochemical capacitance performance is not as good as embodiment 1.
Table 1. Pr (OH)3The adjusting and controlling growth of nanometer rods
Claims (8)
1. a Pr (OH)3The preparation method of monodimension nano stick, it is characterised in that described preparation method is configuration precursor solution,
Pr (OH) is generated at working electrode surface by step constant current galvanoplastic3Monodimension nano stick；Described precursor solution is praseodymium salt
With the mixed aqueous solution of ammonium salt, in described precursor solution, the concentration of praseodymium salt is (1 ~ 8) g/L；Described praseodymium salt and the mixing of ammonium salt
Than being (1 ~ 7): 1；Described electroplating temperature is 60 ~ 80 DEG C, and electroplating current is 1.5-2 mA；Described electroplating time is 1 ~ 3h.
Preparation method the most according to claim 1, it is characterised in that in described precursor solution, the concentration of praseodymium salt is
4.5g/L；The mixing ratio of described praseodymium salt and ammonium salt is 3:1.
Preparation method the most according to claim 1, it is characterised in that described electroplating temperature is 70 DEG C, electroplating current is 2
mA；Described electroplating time is 2h.
Preparation method the most according to claim 1, it is characterised in that described praseodymium salt is praseodymium nitrate, described ammonium salt is nitric acid
Ammonium.
Preparation method the most according to claim 1, it is characterised in that described working electrode is conduction carbon cloth, metallic conduction
Material or conduction FTO glass.
The most according to claim 1 or 5, preparation method, it is characterised in that described working electrode is titanium sheet, platinum electrode is right
Electrode.
7. the Pr (OH) that the preparation method described in a claim 1 to 6 prepares31-dimention nano bar material.
8. the Pr (OH) described in claim 73The application in energy storage of the 1-dimention nano bar material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610455969 | 2016-06-22 | ||
| CN2016104559697 | 2016-06-22 |
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| JPS62132731A (en) * | 1985-12-03 | 1987-06-16 | Seitetsu Kagaku Co Ltd | Production of rare earth metal oxide |
| CN1403375A (en) * | 2002-10-11 | 2003-03-19 | 清华大学 | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide |
| JP2003197462A (en) * | 2001-12-28 | 2003-07-11 | Murata Mfg Co Ltd | Method of manufacturing laminated ceramic electronic component |
| CN1800026A (en) * | 2005-12-23 | 2006-07-12 | 浙江大学 | Microwave synthesis preparation method for praseodymium hydroxide nanometer rod |
| CN101624206A (en) * | 2009-08-07 | 2010-01-13 | 南开大学 | Preparation method and application of rare earth metal hydroxide or vanadate nano material |
| CN102251266A (en) * | 2011-07-07 | 2011-11-23 | 北京工业大学 | Method for preparing nano platinum/titanium dioxide nanotube electrode by pulse electrodeposition |
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2016
- 2016-07-25 CN CN201610587957.XA patent/CN106241852A/en active Pending
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