CN109036870A - A kind of preparation method of niobium pentaoxide and niobium combination electrode - Google Patents
A kind of preparation method of niobium pentaoxide and niobium combination electrode Download PDFInfo
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- CN109036870A CN109036870A CN201811038430.7A CN201811038430A CN109036870A CN 109036870 A CN109036870 A CN 109036870A CN 201811038430 A CN201811038430 A CN 201811038430A CN 109036870 A CN109036870 A CN 109036870A
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- China
- Prior art keywords
- niobium
- preparation
- combination electrode
- pentaoxide
- ultrapure water
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- 239000010955 niobium Substances 0.000 title claims abstract description 33
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 25
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 18
- 239000012498 ultrapure water Substances 0.000 claims abstract description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- YTPZWYPLOCEZIX-UHFFFAOYSA-N [Nb]#[Nb] Chemical compound [Nb]#[Nb] YTPZWYPLOCEZIX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 7
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000002000 scavenging effect Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 239000011230 binding agent Substances 0.000 abstract description 4
- 239000011149 active material Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 6
- 239000007772 electrode material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
Classifications
-
- 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
- H01G11/46—Metal oxides
-
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
-
- 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)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
The invention discloses the preparation methods of a kind of niobium pentaoxide and niobium combination electrode, which is characterized in that the preparation method includes the steps that following: it is stand-by that niobium niobium sheet (1) being cleaned by ultrasonic to drying in acetone, dehydrated alcohol, ultrapure water；(2) ammonium hydroxide, hydrogen peroxide, ultrapure water are measured, is uniformly mixed and obtains solution；(3) solution in step (2) is gone in the polytetrafluoroethyllining lining of autoclave, then the niobium sheet in step (1) is fixed in the solution, it after stainless steel casing is sealed, puts and heats in an oven, so that it may obtain niobium pentaoxide/niobium combination electrode.Its step is less first, method is simpler compared to common process by preparation process of the invention；Secondly the binding force of active material and matrix is higher, is conducive to the cyclical stability for improving electrode；Finally due to not having the addition of insulating properties binder, it is more suitable for high current working characteristics.
Description
Technical field
The present invention relates to electrode technology fields, are related specifically to the preparation side of a kind of niobium pentaoxide and niobium combination electrode
Method.
Background technique
Compared to conventional rechargeable, supercapacitor has the characteristics that oneself is exclusive for the demand of electrode material,
As we know that the charge and discharge of conventional rechargeable are realized by the redox reaction of positive and negative pole material.Its work
Principle and supercapacitor have significant difference.So the requirement for also having its different on electrode material.Niobium pentaoxide
(Nb2O5) it is a kind of noticeable electrode material, and it is based on Nb2O5The electrode of material has excellent performance of the supercapacitor,
Therefore become a kind of important electrode.Simultaneously as the performance of electrode is largely dependent upon preparation method, therefore have
Very crucial effect.The method that the prior art generally uses is to prepare Nb2O5 powder first, then dry by grinding-pasting-
The techniques such as dry, whole process is many and diverse, and time-consuming and laborious, simultaneously because the addition of the binder of insulating properties, causes electrode working
When can generate a large amount of heat, not only will cause larger energy consumption, and will cause potential danger, this point high current work when
It can be more significant.
Summary of the invention
Technical problems to be solved: the purpose of the present invention is to provide the present invention is directed to propose a kind of Nb2O5Electrode it is simple
Preparation method not only avoids the process that powder body material prepares electrode, and can improve to avoid the addition of insulating properties binder
The conductivity of electrode, to provide a kind of simple preparation method of electrode for being conducive to high power work.
Technical solution: to solve the above-mentioned problems, the invention discloses a kind of preparations of niobium pentaoxide/niobium combination electrode
Method, the preparation method include the steps that following:
(1) niobium niobium sheet is cut into the small pieces of 1*2cm, is then cleaned by ultrasonic in acetone, dehydrated alcohol, ultrapure water respectively
It 10-30 minutes, is then dried with nitrogen stand-by；
(2) ammonium hydroxide, hydrogen peroxide, ultrapure water are measured, is uniformly mixed and obtains solution；
(3) solution in step (2) is gone in the polytetrafluoroethyllining lining of autoclave, then by the niobium in step (1)
Piece is fixed in the solution, after stainless steel casing is sealed, after putting 150-200 DEG C of heat treatment 1-3h in an oven, so that it may
To niobium pentaoxide/niobium combination electrode.
Preferably, scavenging period is 15min in the step (1).
Preferably, ammonium hydroxide in the step (2), hydrogen peroxide, ultrapure water mass ratio be 1-5:10-20:10-20.
It is further preferred that the mass ratio of ammonium hydroxide in the step (2), hydrogen peroxide, ultrapure water is 1-5:20:20.
Preferably, heat at 170-190 DEG C in an oven in the step (3).
Preferably, heat 2h in an oven in the step (3).
Compared with prior art, the present invention has the advantages that: preparation process of the invention is first compared to common process
Its step is less, method is simpler；Secondly the binding force of active material and matrix is higher, and the circulation for being conducive to improve electrode is steady
It is qualitative；Finally due to not having the addition of insulating properties binder, it is more suitable for high current working characteristics.
Detailed description of the invention
Fig. 1 is porous Nb prepared by the surface Nb of embodiment 12O5Porous electrode；
Fig. 2 is porous Nb prepared by the surface Nb of embodiment 22O5Porous electrode；
Fig. 3 is porous Nb prepared by the surface Nb of embodiment 32O5Porous electrode；
Fig. 4 is porous Nb prepared by the surface Nb of embodiment 42O5Porous electrode.
Specific embodiment
Embodiment 1
(1) niobium niobium sheet is cut into the small pieces of 1*2cm, is then cleaned by ultrasonic 15 in acetone, dehydrated alcohol, ultrapure water respectively
Minute, it is then dried with nitrogen stand-by；
(2) ammonium hydroxide, 20ml hydrogen peroxide, the 20ml ultrapure water for measuring 1ml, are uniformly mixed and obtain solution；
(3) solution in (2) is gone in the polytetrafluoroethyllining lining of autoclave, is then fixed on the niobium sheet in (1)
In solution.After stainless steel casing is sealed, after putting 180 DEG C of heat treatment 2h in an oven, so that it may obtain niobium pentaoxide/niobium
Combination electrode, as shown in Figure 1.
Embodiment 2
(1) niobium niobium sheet is cut into the small pieces of 1*2cm, is then cleaned by ultrasonic 15 in acetone, dehydrated alcohol, ultrapure water respectively
Minute, it is then dried with nitrogen stand-by；
(2) ammonium hydroxide, 20ml hydrogen peroxide, the 20ml ultrapure water for measuring 5ml, are uniformly mixed and obtain solution；
(3) solution in step (2) is gone in the polytetrafluoroethyllining lining of autoclave, then by the niobium in step (1)
Piece is fixed in the solution；After stainless steel casing is sealed, after putting 180 DEG C of heat treatment 2h in an oven, so that it may obtain five oxygen
Change two niobiums/niobium combination electrode, as shown in Figure 2.
Embodiment 3
(1) niobium niobium sheet is cut into the small pieces of 1*2cm, is then cleaned by ultrasonic 15 in acetone, dehydrated alcohol, ultrapure water respectively
Minute, it is then dried with nitrogen stand-by；
(2) ammonium hydroxide, 20ml hydrogen peroxide, the 20ml ultrapure water for measuring 40ml, are uniformly mixed and obtain solution；
(3) solution in (2) is gone in the polytetrafluoroethyllining lining of autoclave, is then fixed on the niobium sheet in (1)
In solution.After stainless steel casing is sealed, after putting 180 DEG C of heat treatment 2h in an oven, so that it may obtain niobium pentaoxide/niobium
Combination electrode, as shown in Figure 3.
Embodiment 4
(1) niobium niobium sheet is cut into the small pieces of 1*2cm, is then cleaned by ultrasonic 15 in acetone, dehydrated alcohol, ultrapure water respectively
Minute, it is then dried with nitrogen stand-by；
(2) 20ml hydrogen peroxide, 20ml ultrapure water are measured, and weighs 0.1g NH4F is added, and is uniformly mixed and obtains solution；
(3) solution in (2) is gone in the polytetrafluoroethyllining lining of autoclave, is then fixed on the niobium sheet in (1)
In solution.After stainless steel casing is sealed, after putting 180 DEG C of heat treatment 2h in an oven, so that it may obtain niobium pentaoxide/niobium
Combination electrode, as shown in Figure 4.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (6)
1. the preparation method of a kind of niobium pentaoxide and niobium combination electrode, which is characterized in that the preparation method includes following
The step of:
(1) niobium niobium sheet is cut into the small pieces of 1*2cm, is then cleaned by ultrasonic 10-30 in acetone, dehydrated alcohol, ultrapure water respectively
Minute, it is then dried with nitrogen stand-by；
(2) ammonium hydroxide, hydrogen peroxide, ultrapure water are measured, is uniformly mixed and obtains solution；
(3) solution in step (2) is gone in the polytetrafluoroethyllining lining of autoclave, it is then that the niobium sheet in step (1) is solid
Determine in the solution, after stainless steel casing is sealed, after putting 150-200 DEG C of heat treatment 1-3h in an oven, so that it may obtain five
Aoxidize two niobiums/niobium combination electrode.
2. the preparation method of a kind of niobium pentaoxide and niobium combination electrode according to claim 1, it is characterised in that described
The step of (1) in scavenging period be 15min.
3. the preparation method of a kind of niobium pentaoxide and niobium combination electrode according to claim 1, it is characterised in that described
The step of (2) in ammonium hydroxide, hydrogen peroxide, ultrapure water mass ratio be 1-5:10-20:10-20.
4. the preparation method of a kind of niobium pentaoxide and niobium combination electrode according to claim 3, it is characterised in that described
The step of (2) in ammonium hydroxide, hydrogen peroxide, ultrapure water mass ratio be 1-5:20:20.
5. the preparation method of a kind of niobium pentaoxide and niobium combination electrode according to claim 3, it is characterised in that described
The step of (3) in heat at 170-190 DEG C in an oven.
6. the preparation method of a kind of niobium pentaoxide and niobium combination electrode according to claim 3, it is characterised in that described
The step of (3) in heat 2h in an oven.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811038430.7A CN109036870A (en) | 2018-09-06 | 2018-09-06 | A kind of preparation method of niobium pentaoxide and niobium combination electrode |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811038430.7A CN109036870A (en) | 2018-09-06 | 2018-09-06 | A kind of preparation method of niobium pentaoxide and niobium combination electrode |
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| CN109036870A true CN109036870A (en) | 2018-12-18 |
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| CN201811038430.7A Withdrawn CN109036870A (en) | 2018-09-06 | 2018-09-06 | A kind of preparation method of niobium pentaoxide and niobium combination electrode |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288134A (en) * | 2013-05-14 | 2013-09-11 | 西南交通大学 | Preparation method of spindle niobium oxides |
| CN106206077A (en) * | 2016-06-30 | 2016-12-07 | 江苏大学 | A kind of preparation method and its usage of nanometer niobium pentaoxide/FTO aqueous super capacitor electrode material |
| CN108479790A (en) * | 2018-04-10 | 2018-09-04 | 北京化工大学 | A kind of multistage Core-shell structure material and preparation method thereof |
-
2018
- 2018-09-06 CN CN201811038430.7A patent/CN109036870A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288134A (en) * | 2013-05-14 | 2013-09-11 | 西南交通大学 | Preparation method of spindle niobium oxides |
| CN106206077A (en) * | 2016-06-30 | 2016-12-07 | 江苏大学 | A kind of preparation method and its usage of nanometer niobium pentaoxide/FTO aqueous super capacitor electrode material |
| CN108479790A (en) * | 2018-04-10 | 2018-09-04 | 北京化工大学 | A kind of multistage Core-shell structure material and preparation method thereof |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181218 |
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| WW01 | Invention patent application withdrawn after publication |