CN106898496A - The preparation method and application of the bullet-shaped cobalt phosphate nickel ammonium particulate with multilayer scale - Google Patents
The preparation method and application of the bullet-shaped cobalt phosphate nickel ammonium particulate with multilayer scale Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The preparation method and application of the bullet-shaped cobalt phosphate nickel ammonium particulate with multilayer scale, belong to material, chemosynthesis technical field, ammonium phosphate, Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate, deionized water, ethylene glycol are mixed, reaction mixture is obtained, being placed in after ultrasonic disperse carries out hydro-thermal reaction in reactor；Then the system after hydro-thermal reaction is cooled to room temperature, taking precipitate is washed with water and ethanol, dried, and obtains the bullet-shaped cobalt phosphate nickel ammonium particulate with multilayer scale.Simple to operate, environmentally friendly, product grain of the invention is uniform in size, specific surface area is larger, and distributivity is good, and material can be used for the fields such as ultracapacitor, battery and electro-catalysis.
Description
Technical field
The invention belongs to material, chemosynthesis technical field, more particularly to cobalt phosphate nickel ammonium material alcohol auxiliary water heat seal
Into method and its application.
Background technology
At present, iron system phosphate micro Nano material is extensive because species is various, Stability Analysis of Structures, electrochemical behavior enrich
Apply in every field such as electrochemical energy storage, adsorbent, catalyst, carriers.Especially composition metal phosphate material, due to it
The features such as Stability Analysis of Structures, electrochemical behavior enrich, they are paid close attention to frequently as electrochemical energy storage materials by many scientists.
But composition metal phosphate material synthesis condition is harsh, high temperature, inert gas shielding the need for having.Other high temperature
Under the conditions of synthesize particle size, the mutually bad control of thing, have a strong impact on its electrochemical energy storage performance.How to close in a mild condition
Into size uniform, thing be mutually single, excellent performance electrochemical energy storage materials are a urgent problems.And function nano
The property of material is not only relevant with its size, but also relevant with its pattern, micro nano structure, the gold of all kinds of micro nano structures
Category phosphate material has different micro-nano surface and interface properties, therefore is demonstrated by many peculiar physicochemical properties.
The content of the invention
It is an object of the present invention to provide easy to operate, the free of contamination alcohol assisted hydrothermal synthesis method of one kind, the method can synthesize
Go out that pattern is homogeneous, and the multilayer scale bullet-shaped cobalt phosphate nickel ammonium nano material with large specific surface area.
Preparation method of the invention is comprised the following steps：
1）Ammonium phosphate, Nickelous nitrate hexahydrate and cabaltous nitrate hexahydrate are mixed with deionized water and ethylene glycol and is reacted, obtained
Reaction mixture；
2）Reaction mixture is ultrasonically treated, obtain finely dispersed mixed system；
3）Finely dispersed mixed system is placed in carries out hydro-thermal reaction in reactor；
4）System after hydro-thermal reaction is cooled to room temperature, precipitation is obtained, then is washed with water and ethanol, dried, obtained with many
The bullet-shaped cobalt phosphate nickel ammonium particulate of layer scale.
Because the water vapour in cabaltous nitrate hexahydrate and the easy absorption air of Nickelous nitrate hexahydrate, therefore reaction need to be added
Carried out in ionized water and ethylene glycol.The present invention has strong coordination using the hydroxyl of alcohol, is allowed to form cooperation with metal ion
Thing, some crystal faces in nucleus are adsorbed by it, limit the growth of some crystal faces so as to control synthesis with special grain boundary surface
Micro nano structure, the pattern of the bullet-shaped with multilayer scale is formed with this.
Simple to operate, environmentally friendly, product grain of the invention is uniform in size, specific surface area is larger, and distributivity is good, and entirely
Building-up process is easy to operation, clean and safe.Bullet-shaped cobalt phosphate nickel ammonium material with multilayer scale prepared by the present invention
Material can be used for the fields such as ultracapacitor, battery and electro-catalysis.
Further, nickel nitrate rubs with the mixing of cobalt nitrate in cabaltous nitrate hexahydrate in Nickelous nitrate hexahydrate of the present invention
You are than being 4~7.5: 1.Cobalt element is adulterated on a small quantity, be more beneficial for two kinds of metallic elements and form single-phase, stabilization answering
Close metal phosphate material.
The ammonium phosphate is 3: 2~3 with the mixing quality ratio of Nickelous nitrate hexahydrate.Under the proportioning, ammonium phosphate relative to
Nickelous nitrate hexahydrate is slightly excessive, preferably can therewith form complex, and be conducive to a small amount of cobalt element to adulterate wherein.
The Nickelous nitrate hexahydrate and deionized water, the mixing ratio of ethylene glycol are 1mmol: 10ml: 10ml.Technique profit
There is strong coordination with the hydroxyl of alcohol, be allowed to form complex with metal ion, and by adsorbing some crystalline substances in nucleus
Face, limits the growth of some crystal faces so as to control micro nano structure of the synthesis with special grain boundary surface.In addition, ethylene glycol and going
The volume ratio of ionized water is about 1: 1, and using the weak reducing power of alcohol, can protect under certain condition phosphatic micro-nano
Structure.
Another object of the present invention also proposes that the above has the purposes of the bullet-shaped cobalt phosphate nickel ammonium particulate of multilayer scale.
There is the bullet-shaped cobalt phosphate nickel ammonium particulate of multilayer scale to be applied to make the electrode of ultracapacitor by more than
Material.
After tested, in 0.5 A g-1Current density under, the specific capacitance of electrode is up to 540.8 F g-1.In 10 A g-1
High current density under, specific capacity still maintains 83.9% or so.
It can be seen that, the bullet-shaped cobalt nickel composite phosphate particulate with multilayer scale of the invention is in catalysis, battery, photon
The aspects such as device also have broad application prospects.This alcohol auxiliary hydrothermal preparing process can also promote micro- for other simultaneously
The controlledly synthesis of nano material.
Brief description of the drawings
The ESEM of the product of Fig. 1 embodiment of the present invention 1（SEM）Figure.
The SEM figures of the product of Fig. 2 embodiment of the present invention 2.
The SEM figures of the product of Fig. 3 embodiment of the present invention 3.
The SEM figures of the product of Fig. 4 embodiment of the present invention 4.
The SEM figures of the product of Fig. 5 embodiment of the present invention 5.
SEM figure of the product of Fig. 6 embodiment of the present invention 5 under low range.
The SEM figures of the product of Fig. 7 embodiment of the present invention 6.
The X-ray diffraction of the product of Fig. 8 embodiment of the present invention 5（XRD）Collection of illustrative plates.
The constant current charge-discharge of the product of Fig. 9 embodiment of the present invention 5（CP）Curve.
Specific embodiment：
In order to be better understood from the present invention, with reference to embodiment, the present invention is described further.
First, preparation technology：
Embodiment 1：
(1) 0.3 g ammonium phosphate, 0.24 g Nickelous nitrate hexahydrates and 0.06 g cabaltous nitrate hexahydrates are weighed respectively, all pour into 10
In mL deionized waters and 10 mL ethylene glycol, mixed liquor is stirred at room temperature uniformly, is allowed to well mixed and fully reacts.
Nickel nitrate and the mixing mol ratio of cobalt nitrate are 4: 1 in above materials.
(2) the reacted mixed system of upper step is put into ultrasound in ultrasonic machine, makes each component dispersed.
(3) hydro-thermal reaction is carried out at dispersed system then being placed on into 200 DEG C 45 hours.
(4) after hydro-thermal reaction terminates, after reaction solution is naturally cooled into room temperature, reactant is taken out, through stratification, is obtained
Precipitation, then washed with water and ethanol, then dry, obtain bluish grey cobalt phosphate nickel ammonium powder.
Embodiment 2：
(1) 0.3 g ammonium phosphate, 0.24 g Nickelous nitrate hexahydrates and 0.06 g cabaltous nitrate hexahydrates are weighed respectively, all pour into 10
In mL deionized waters and 10 mL ethylene glycol, mixed liquor is stirred at room temperature uniformly, is allowed to well mixed and fully reacts.
(2) the reacted mixed system of upper step is put into ultrasound in ultrasonic machine, makes each component dispersed.
(3) hydro-thermal reaction is carried out at dispersed system then being placed on into 200 DEG C 20 hours.
(4) after hydro-thermal reaction terminates, after reaction solution is naturally cooled into room temperature, reactant is taken out, through stratification, is obtained
Precipitation, then washed with water and ethanol, then dry, obtain bluish grey cobalt phosphate nickel ammonium powder.
Embodiment 3：
(1) 0.3 g ammonium phosphate, 0.3g Nickelous nitrate hexahydrates and 0.04g cabaltous nitrate hexahydrates are weighed respectively, all pour into 10 mL
In deionized water and 10 mL ethylene glycol, mixed liquor is stirred at room temperature uniformly, is allowed to well mixed and fully reacts.
Nickel nitrate and the mixing mol ratio of cobalt nitrate are 7.5: 1 in above materials.
(2) the reacted mixed system of upper step is put into ultrasound in ultrasonic machine, makes each component dispersed.
(3) hydro-thermal reaction is carried out at dispersed system then being placed on into 200 DEG C 10 hours.
(4) after hydro-thermal reaction terminates, after reaction solution is naturally cooled into room temperature, reactant is taken out, through stratification, is obtained
Precipitation, then washed with water and ethanol, then dry, obtain bluish grey cobalt phosphate nickel ammonium powder.
Embodiment 4：
(1) 0.3 g ammonium phosphate, 0.3g Nickelous nitrate hexahydrates and 0.04g cabaltous nitrate hexahydrates are weighed respectively, all pour into 10 mL
In deionized water and 10 mL ethylene glycol, mixed liquor is stirred at room temperature uniformly, is allowed to well mixed and fully reacts.
(2) the reacted mixed system of upper step is put into ultrasound in ultrasonic machine, makes each component dispersed.
(3) hydro-thermal reaction is carried out at dispersed system then being placed on into 160 DEG C 20 hours.
(4) after hydro-thermal reaction terminates, after reaction solution is naturally cooled into room temperature, reactant is taken out, through stratification, is obtained
Precipitation, then washed with water and ethanol, then dry, obtain bluish grey cobalt phosphate nickel ammonium powder.
Embodiment 5：
(1) 0.3 g ammonium phosphate, 0.3g Nickelous nitrate hexahydrates and 0.04g cabaltous nitrate hexahydrates are weighed respectively, all pour into 10 mL
In deionized water and 10 mL ethylene glycol, mixed liquor is stirred at room temperature uniformly, is allowed to well mixed and fully reacts.
(2) the reacted mixed system of upper step is put into ultrasound in ultrasonic machine, makes each component dispersed.
(3) hydro-thermal reaction is carried out at dispersed system then being placed on into 200 DEG C 20 hours.
(4) after hydro-thermal reaction terminates, after reaction solution is naturally cooled into room temperature, reactant is taken out, through stratification, is obtained
Precipitation, then washed with water and ethanol, then dry, obtain bluish grey cobalt phosphate nickel ammonium powder.
Embodiment 6：
(1) 0.3 g ammonium phosphate, 0.3g Nickelous nitrate hexahydrates and 0.04g cabaltous nitrate hexahydrates are weighed respectively, all pour into 10 mL
In deionized water and 10 mL ethylene glycol, mixed liquor is stirred at room temperature uniformly, is allowed to well mixed and fully reacts.
(2) the reacted mixed system of upper step is put into ultrasound in ultrasonic machine, makes each component dispersed.
(3) hydro-thermal reaction is carried out at dispersed system then being placed on into 200 DEG C 40 hours.
(4) after hydro-thermal reaction terminates, after reaction solution is naturally cooled into room temperature, reactant is taken out, through stratification, is obtained
Precipitation, then washed with water and ethanol, then dry, obtain bluish grey cobalt phosphate nickel ammonium powder.
2nd, result verification：
Fig. 1 is the SEM figures of cobalt phosphate nickel ammonium composite particles prepared by embodiment 1.Fig. 1 shows that particle is presented the smooth son in surface
Bullet pattern, specific surface area is smaller, but the reaction time is more long, consumes energy larger.
Fig. 2 is the SEM figures of cobalt phosphate nickel ammonium composite particles prepared by embodiment 2.Fig. 2 shows the major diameter of sub warhead particle
Decline than, but occur in that a small amount of flaky mixture, illustrated that partial reaction thing does not react fully, influence its performance.
Fig. 3 is the SEM figures of cobalt phosphate nickel ammonium composite particles prepared by embodiment 3, and Fig. 3 shows the table of bullet-shaped particle
Face starts a small amount of nanometer scale occur, and the specific surface area of particle increases, but its granular size disunity, and distribution is also uneven
It is even, illustrate that the amount adulterated by increasing nickel can make microparticle surfaces structure change, but reaction is not carried out completely.
Fig. 4 is the SEM figures of cobalt phosphate nickel ammonium composite particles prepared by embodiment 4, and Fig. 4 shows the table of bullet-shaped particle
There is a small amount of plane defect in face, and granular size disunity, distribution is also uneven, around there is a small amount of impurity, illustrates when temperature is relatively low
Reaction can not be carried out completely.
Fig. 5 is the SEM figures of cobalt phosphate nickel ammonium particle prepared by embodiment 5.Fig. 5 shows that particle surface is covered with substantial amounts of receiving
Rice scale, can improve its specific surface area, improve the interface performance of material, and the simultaneous reactions time is shorter, with respect to energy-conservation.
Fig. 6 is the SEM figures under the sample low range of embodiment 5.Fig. 6 shows that granule-morphology is unified, uniform in size, illustrates this
Carried out under reaction controlled condition, and reaction can be carried out fully.It can be seen that, embodiment 5 is used for preferably embodiment.
Fig. 7 is the SEM figures of cobalt phosphate nickel ammonium composite particles prepared by embodiment 6.Fig. 7 starts mutually between showing particle
Fusion, it is long between illustrating when reacted to cause overreact.
Fig. 8 is the XRD of the product of embodiment 5, and the diffraction maximum at 2 theta is contrasted with standard crystal card, is sent out
The crystallographic plane diffraction peak of the product of current embodiment 5 and (NH4)(Ni,Co)PO4Diffraction maximum it is basically identical, show the bullet-shaped particulate
It is cobalt phosphate nickel ammonium.
Fig. 9 is the cobalt phosphate nickel ammonium composite particles obtained using embodiment 5 as charge and discharge during electrode material for super capacitor
Electric curve map.
3rd, concrete application：
After sample drying prepared by embodiment 5, grinding 30 minutes or so in agate mortar is put into, and add appropriate isopropanol again
Grinding 20 minutes or so, adds adhesive PTFE (polytetrafluoroethylene (PTFE)), continues to grind 10 minutes or so, by mixture with once
Property dropper drop in size be 1 × 5 centimetre rectangle foam nickel sheet foremost, mixture area is about 1 × 1 centimetre.Again will
The electrode slice made is put into drying for one day left and right in baking oven.
Electrode slice is carried out into compressing tablet after taking-up, is weighed.The electrode slice that will be made again is assembled into three-electrode system and carries out performance
Test, electrolyte is the potassium hydroxide solution of 3M.
After measured, the sample of embodiment 5 shows excellent chemical property as electrode material for super capacitor.Such as Fig. 9
It is shown：In 0.5 A g-1Current density under specific capacitance reach 540.8 F g-1.In addition, the sample is in different current densities
(1 A g-1, 2 A g-1, 5 A g-1, 10 A g-1) under specific capacity be respectively 525.6 F g-1, 518.0 F g-1, 453.8
F g-1, 441.0 F g-1.It is worth noting that, in 10 A g-1High current density under, the specific capacity of this sample is still maintained
83.9% or so, show good high rate performance.
Claims (6)
1. there is the preparation method of the bullet-shaped cobalt phosphate nickel ammonium particulate of multilayer scale, it is characterised in that comprise the following steps：
1）Ammonium phosphate, Nickelous nitrate hexahydrate and cabaltous nitrate hexahydrate are mixed with deionized water and ethylene glycol and is reacted, obtained
Reaction mixture；
2）Reaction mixture is ultrasonically treated, obtain finely dispersed mixed system；
3）Finely dispersed mixed system is placed in carries out hydro-thermal reaction in reactor；
4）System after hydro-thermal reaction is cooled to room temperature, precipitation is obtained, then is washed with water and ethanol, dried, obtained with many
The bullet-shaped cobalt phosphate nickel ammonium particulate of layer scale.
2. preparation method according to claim 1, it is characterised in that：Nickel nitrate and six hydrations in the Nickelous nitrate hexahydrate
The mixing mol ratio of cobalt nitrate is 4~7.5: 1 in cobalt nitrate.
3. preparation method according to claim 2, it is characterised in that：The mixing matter of the ammonium phosphate and Nickelous nitrate hexahydrate
Amount is than being 3: 2~3.
4. the preparation method according to claim 1 or 2 or 3, it is characterised in that：The Nickelous nitrate hexahydrate and deionization
Water, the mixing ratio of ethylene glycol are 1mmol: 10ml: 10ml.
5. preparation method according to claim 1, it is characterised in that：The temperature conditionss of the hydro-thermal reaction be 200 DEG C at,
Reaction time is 20 hours.
6. as the bullet-shaped cobalt phosphate nickel ammonium particulate with multilayer scale prepared by claim 1 method can be applied to make super
The electrode material of level capacitor.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108609599A (en) * | 2018-05-30 | 2018-10-02 | 北京化工大学常州先进材料研究院 | The preparation method of nickel hydroxide nano piece self assembly nickel phosphates cobalt club shaped structure composite material |
| CN109851955A (en) * | 2019-03-13 | 2019-06-07 | 河北大学 | A kind of flame retarding PVC composition for cable and preparation method thereof |
| CN110359271A (en) * | 2019-08-23 | 2019-10-22 | 浙江理工大学 | A kind of cobalt nickel bimetal hydroxyl phosphite flat crystal film and preparation method thereof |
| CN110918113A (en) * | 2019-10-16 | 2020-03-27 | 西南交通大学 | Method for preparing cobalt-nickel-ammonium phosphate catalyst by using ammonia nitrogen wastewater and simulation experiment method |
| CN113161542A (en) * | 2020-12-10 | 2021-07-23 | 三峡大学 | Cathode material of water-based zinc-cobalt battery |
| CN113990675A (en) * | 2021-09-30 | 2022-01-28 | 南京大学 | CoPi/BiVO for high-performance solar charging device4Faraday photoelectrode material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108609599A (en) * | 2018-05-30 | 2018-10-02 | 北京化工大学常州先进材料研究院 | The preparation method of nickel hydroxide nano piece self assembly nickel phosphates cobalt club shaped structure composite material |
| CN109851955A (en) * | 2019-03-13 | 2019-06-07 | 河北大学 | A kind of flame retarding PVC composition for cable and preparation method thereof |
| CN110359271A (en) * | 2019-08-23 | 2019-10-22 | 浙江理工大学 | A kind of cobalt nickel bimetal hydroxyl phosphite flat crystal film and preparation method thereof |
| CN110359271B (en) * | 2019-08-23 | 2021-08-03 | 浙江理工大学 | Cobalt-nickel bimetallic hydroxyl phosphite sheet crystal film and preparation method thereof |
| CN110918113A (en) * | 2019-10-16 | 2020-03-27 | 西南交通大学 | Method for preparing cobalt-nickel-ammonium phosphate catalyst by using ammonia nitrogen wastewater and simulation experiment method |
| CN110918113B (en) * | 2019-10-16 | 2021-03-30 | 西南交通大学 | Method for preparing cobalt-nickel-ammonium phosphate catalyst by using ammonia nitrogen wastewater and simulation experiment method |
| CN113161542A (en) * | 2020-12-10 | 2021-07-23 | 三峡大学 | Cathode material of water-based zinc-cobalt battery |
| CN113161542B (en) * | 2020-12-10 | 2024-03-15 | 三峡大学 | Water-based zinc-cobalt battery positive electrode material |
| CN113990675A (en) * | 2021-09-30 | 2022-01-28 | 南京大学 | CoPi/BiVO for high-performance solar charging device4Faraday photoelectrode material and preparation method thereof |
| CN113990675B (en) * | 2021-09-30 | 2023-01-06 | 南京大学 | CoPi/BiVO for high-performance solar charging device 4 Faraday photoelectrode material and preparation method thereof |
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