CN102502786A - Method for preparing cadmium hydroxide nanowires - Google Patents
Method for preparing cadmium hydroxide nanowires Download PDFInfo
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- CN102502786A CN102502786A CN2011103192616A CN201110319261A CN102502786A CN 102502786 A CN102502786 A CN 102502786A CN 2011103192616 A CN2011103192616 A CN 2011103192616A CN 201110319261 A CN201110319261 A CN 201110319261A CN 102502786 A CN102502786 A CN 102502786A
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Abstract
The invention provides a method for preparing cadmium hydroxide nanowires. The method comprises the following steps of: 1, performing ultrasonic cleaning on a pure copper sheet by using acetone; 2, putting the cleaned pure copper sheet into a container with a mixed solution of benzene and cadmium nitrate; 3, slowly adding a 0.5mol/L sodium hydroxide solution into the container; and 4, reacting at room temperature for 48 hours, taking a precipitate out, cleaning by using distilled water and absolute ethanol in turn, and drying in air to obtain the cadmium hydroxide nanowires. The method for synthesizing the cadmium hydroxide nanowires is simple and practicable, low in cost, high in repeatability, mild in preparation conditions and favorable for large-scale industrial production, a surfactant or a template is not used, and products have uniform appearance. The cadmium hydroxide nanowires prepared by the method can greatly improve the capacity of a nickel-cadmium battery.
Description
Technical field
That the present invention relates to is a kind of preparation method of nickel-cadmium cell cathode material.Specifically a kind of preparation method who is mainly used in the cadmium hydroxide nano wire of nickel-cadmium cell cathode material.
Background technology
Since 19th century, nickel-cadmium cell was invented, be widely used in the various device.But the advantage of nickel-cadmium cell is long charge and discharge cycles of life-span 500～1000 times, physical strength height, good seal performance, use temperature wide ranges (40～+ 50 ℃), method of use is simple, maintaining is convenient, safe and reliable, can tolerate the temporary impact of big electric current (be higher than normal use electric current several times and even 10 times) and do not damage, in normal work period, sustaining voltage is very stable for a long time.Because above advantage, nickel-cadmium cell have obtained using widely.The preparation method of nickel-cadmium cell cathode material in the past mainly be different chemical process for example: chemical bath deposition, the absorption of successive particle and desorb, electrodip process etc. are applied in the preparation of cadmium hydroxide nanostructure.Main challenge in the future development of nickel-cadmium cell will be referred under harsh working conditions, to have the heavy-current discharge characteristic, higher capacity and longer weather resistance.In nickel-cadmium cell; Because the formed defective of exchange of cadmium hydroxide and cadmium metal can influence the capacity of battery; And the discharging that increases the toxic heavy metal cadmium pollutes the environment, and the new cadmium hydroxide electrode materials of therefore inventing a kind of heavy body has important academic significance and use value.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of cadmium hydroxide nano wire of the capacity that can increase substantially nickel-cadmium cell.
The objective of the invention is to realize like this:
The first step: the fine copper sheet is carried out ultrasonic cleaning with acetone;
Second step: the fine copper sheet after the cleaning places the container that benzene and cadmium nitrate mixing solutions are housed; The 0.1mol/L cadmium nitrate solution that consists of 10mL benzene: 50mL of said benzene and cadmium nitrate mixing solutions; The proportionlity of fine copper sheet and benzene and cadmium nitrate mixing solutions is that every 100ml mixing solutions adds 10cm
2The fine copper sheet;
The 3rd step: in container, slowly add the sodium hydroxide solution of 0.5mol/L, add-on is that every 100ml benzene and cadmium nitrate mixing solutions add 10mL;
The 4th step: after at room temperature reacting 48 hours, take out deposition, clean with zero(ppm) water earlier, clean with absolute ethyl alcohol again, after in air, drying, get final product the cadmium hydroxide nano wire.
The invention provides a kind of tensio-active agent or template do not used, simple for process, cost is low, good reproducibility, preparation condition gentleness, uniform product appearance, help forming the compound method of the cadmium hydroxide nano wire of large-scale industrial production.The cadmium hydroxide nano wire that obtains through this method can increase substantially the capacity of nickel-cadmium cell.
Cadmium hydroxide has unique optics, photoelectronics and catalytic performance as a kind of important functional material, is widely used in fields such as solar cell, battery cathode material, transmitter, transparency electrode, optical transistor and diodes.Cadmium hydroxide has increased the loading capacity of nickel/cadmium cell on the one hand usually as the additive of electrode materials, has reduced the self-discharge of battery itself on the other hand.The present invention has mainly prepared nanometer cadmium hydroxide powder body material and it has been done charge-discharge test.Through test, this bill of material reveals very high capacity and good cyclical stability.
Nano material through method of the present invention obtains is carried out charge-discharge test as nickel-cadmium battery negative pole, shows very high capacity and stability.Change reaction conditions, obtain the cadmium hydroxide nanostructure of different-shape, the cadmium hydroxide of different-shape is carried out charge-discharge test, test result shows, capacity and stability with cadmium hydroxide nano materials of nano thread structure is better than other patterns.
The test that discharges and recharges:
Electrochemical test is carried out through following method:
The cadmium hydroxide nano wire that obtains aforesaid method is being pressed on the nickel foam sheet under the pressure of 50MP.Experimental system is a three-electrode system, and in the KOH solution that 25 ℃ of standard atmospheres are depressed at 5mol/L, carries out, and the cadmium hydroxide nanostructure is a working electrode, Ni (OH)
2/ NiOOH is as counter electrode, and Ag/AgCl is as reference electrode, and all electro-chemical tests all use blue battery system.Through observation to charging and discharging curve; Along with the increase of electrochemistry capacitance, electromotive force is increased to 1.5V, it should be noted that discharge process to the last still remains on 1.25V; Shown a very smooth platform of putting, this has shown that the cadmium hydroxide nano wire has extraordinary discharge stability.Be to circulate 100 times under the 30mA/g in charging and discharging currents density afterwards, the loading capacity of cadmium hydroxide nano wire still is about 220mAh/g.The prepared nickel-cadmium cell of this explanation has good cyclical stability.
Compare the cadmium hydroxide nano wire and have the capacity of the cadmium hydroxide electrode materials (cadmium hydroxide nanoparticle) of different-shape and size through changing resulting other of reaction conditions.Promptly to diameter respectively the nano wire of 100nm, the nanoparticle of 20nm, the nanoparticle of 40nm, its loading capacity of electrochemistry capacitance test shows of the nanoparticle of 500nm is respectively 135mAh/g, 100mAh/g, 100mAh/g and 60mAh/g.Result's proof has proved also that along with the increase capacity of size of particles reduces gradually the form of particle influences their electrochemical stability.Through the contrast of charging and discharging curve, can find out significantly that in electrochemical process, compare with other particles, nano wire has very high capacity and good cyclical stability.
Description of drawings
Fig. 1 a-Fig. 1 d is field emission scan electron microscopic (FE-SEM) image that the present invention tests the cadmium hydroxide nanoparticle that under the differential responses condition, obtains.Wherein Fig. 1 a is the nano wire that the sodium hydroxide solution reaction of 0.1mol/L cadmium nitrate solution and 0.5mol/L obtains; Fig. 1 b is the nanoparticle that 0.1mol/L cadmium nitrate solution and the reaction of 0.1mol/L sodium hydroxide solution obtain; Fig. 1 c is the nanoparticle that 0.5mol/L cadmium nitrate solution and the reaction of 0.1mol/L sodium hydroxide solution obtain; Fig. 1 d is the nanoparticle that 0.5mol/L cadmium nitrate solution and the reaction of 0.5mol/L sodium hydroxide solution obtain.
Fig. 2 a is that the present invention tests resulting cadmium hydroxide nano wire X-ray diffraction (XRD) image; Fig. 2 b is resulting cadmium hydroxide nanometer field of line emission scan electron microscopic (FE-SEM) image for the present invention tests; Fig. 2 c and Fig. 2 d are the loop cycle of charging and discharging curve under the current density of 30mA/g and the cadmium hydroxide nano wire prepared.
Fig. 3 is respectively that diameter is the nano wire of 100nm, the nanoparticle of 20nm, the nanoparticle of 40nm, the charging and discharging curve of the nanoparticle of 500nm.
Embodiment
In order to understand the present invention better, describe through embodiment.
1. the preparation of cadmium hydroxide nano wire:
The first step: get the rectangle fine copper sheet of a 1 * 10cm, copper sheet is carried out ultrasonic cleaning with acetone;
Second step: the 0.1mol/L cadmium nitrate solution of 10mL benzene and 50mL is blended in the beaker of 100ml.
The 3rd step: the sodium hydroxide solution 10mL that in a step solution, slowly adds 0.5mol/L.
The 4th step: beaker is put into stink cupboard, at room temperature react 48 hours after, take out deposition, clean with zero(ppm) water earlier, clean with absolute ethyl alcohol again, after in air, drying, get final product the cadmium hydroxide nano wire.
Embodiment one
This embodiment adopts the solution at room temperature method successfully to prepare the cadmium hydroxide nano wire.
The first step: get the rectangle fine copper sheet of a 1 * 10cm, copper sheet is carried out ultrasonic cleaning with acetone;
Second step: the 0.1mol/L cadmium nitrate solution of 10mL benzene and 50mL is blended in the beaker of 100ml.
The 3rd step: the sodium hydroxide solution 10mL that in a step solution, slowly adds 0.5mol/L.
The 4th step: beaker is put into stink cupboard, at room temperature react 48 hours after, take out deposition, clean with zero(ppm) water earlier, clean with absolute ethyl alcohol again, after in air, drying, get final product the cadmium hydroxide nano wire.
Embodiment two
This embodiment and embodiment one compare
The first step: get the rectangle fine copper sheet of a 1 * 10cm, copper sheet is carried out ultrasonic cleaning with acetone;
Second step: the 0.1mol/L cadmium nitrate solution of 10mL benzene and 50mL is blended in the beaker of 100ml.
The 3rd step: the sodium hydroxide solution 50mL that in a step solution, slowly adds 0.1mol/L.
The 4th step: beaker is put into stink cupboard, at room temperature react 48 hours after, take out deposition, clean with zero(ppm) water earlier, clean with absolute ethyl alcohol again, after in air, drying, get final product the cadmium hydroxide nanoparticle.
Embodiment three
This embodiment and embodiment one compare
The first step: get the rectangle fine copper sheet of a 1 * 10cm, copper sheet is carried out ultrasonic cleaning with acetone;
Second step: the 0.5mol/L cadmium nitrate solution of 10mL benzene and 10mL is blended in the beaker of 100ml.
The 3rd step: the sodium hydroxide solution 50mL that in a step solution, slowly adds 0.1mol/L.
The 4th step: beaker is put into stink cupboard, at room temperature react 48 hours after, take out deposition, clean with zero(ppm) water earlier, clean with absolute ethyl alcohol again, after in air, drying, get final product the cadmium hydroxide nanoparticle.
Embodiment four
This embodiment and embodiment one compare
The first step: get the rectangle fine copper sheet of a 1 * 10cm, copper sheet is carried out ultrasonic cleaning with acetone;
Second step: the 0.5mol/L cadmium nitrate solution of 10mL benzene and 10mL is blended in the beaker of 100ml.
The 3rd step: the sodium hydroxide solution 10mL that in a step solution, slowly adds 0.5mol/L.
The 4th step: beaker is put into stink cupboard, at room temperature react 48 hours after, take out deposition, clean with zero(ppm) water earlier, clean with absolute ethyl alcohol again, after in air, drying, get final product the cadmium hydroxide nanoparticle.
2. the test of charge-discharge performance:
Embodiment one
The diameter that obtains the reaction of the ammoniacal liquor of 0.5mol/L cadmium nitrate solution and PH=13 is that 100nm cadmium hydroxide nano wire is being pressed on the nickel foam sheet under the pressure of 50MP.All experiments all are three-electrode systems, and in the KOH solution that 25 ℃ of standard atmospheres are depressed at 5mol/L, carry out, and the cadmium hydroxide nanostructure is a working electrode, Ni (OH)
2/ NiOOH is as counter electrode, and Ag/AgCl is as reference electrode, and all electro-chemical tests all use blue battery system, is 30mA/g in current density, observes charging and discharging curve.
Embodiment two
The diameter that obtains the reaction of 0.1mol/L cadmium nitrate solution and 0.1mol/L sodium hydroxide solution is that 20nm cadmium hydroxide nano particle is being pressed on the nickel foam sheet under the pressure of 50MP.All experiments all are three-electrode systems, and in the KOH solution that 25 ℃ of standard atmospheres are depressed at 5mol/L, carry out, and the cadmium hydroxide nanostructure is a working electrode, Ni (OH)
2/ NiOOH is as counter electrode, and Ag/AgCl is as reference electrode, and all electro-chemical tests all use blue battery system, is 30mA/g in current density, observes charging and discharging curve.
Embodiment three
The diameter that obtains the reaction of 0.1mol/L cadmium nitrate solution and 0.5mol/L sodium hydroxide solution is that 40nm cadmium hydroxide nano particle is being pressed on the nickel foam sheet under the pressure of 50MP.All experiments all are three-electrode systems, and in the KOH solution that 25 ℃ of standard atmospheres are depressed at 5mol/L, carry out, and the cadmium hydroxide nanostructure is a working electrode, Ni (OH)
2/ NiOOH is as counter electrode, and Ag/AgCl is as reference electrode, and all electro-chemical tests all use blue battery system, is 30mA/g in current density, observes charging and discharging curve.
Embodiment four
The diameter that obtains the reaction of 0.5mol/L cadmium nitrate solution and 0.5mol/L sodium hydroxide solution is that 500nm cadmium hydroxide nano particle is being pressed on the nickel foam sheet under the pressure of 50MP.All experiments all are three-electrode systems, and in the KOH solution that 25 ℃ of standard atmospheres are depressed at 5mol/L, carry out, and the cadmium hydroxide nanostructure is a working electrode, Ni (OH)
2/ NiOOH is as counter electrode, and Ag/AgCl is as reference electrode, and all electro-chemical tests all use blue battery system, is 30mA/g in current density, observes charging and discharging curve.
Above-mentioned resulting charging and discharging curve figure is Fig. 3.
Claims (3)
1. the preparation method of a cadmium hydroxide nano wire is characterized in that:
The first step: the fine copper sheet is carried out ultrasonic cleaning with acetone;
Second step: the fine copper sheet after the cleaning places the container that benzene and cadmium nitrate mixing solutions are housed;
The 3rd step: the sodium hydroxide solution that in container, slowly adds 0.5mol/L;
The 4th step: after at room temperature reacting 48 hours, take out deposition, clean with zero(ppm) water earlier, clean with absolute ethyl alcohol again, after in air, drying, get final product the cadmium hydroxide nano wire.
2. the preparation method of cadmium hydroxide nano wire according to claim 1 is characterized in that: the 0.1mol/L cadmium nitrate solution that consists of 10mL benzene: 50mL of said benzene and cadmium nitrate mixing solutions; The proportionlity of fine copper sheet and benzene and cadmium nitrate mixing solutions is that every 100ml mixing solutions adds 10cm
2The fine copper sheet.
3. the preparation method of cadmium hydroxide nano wire according to claim 1 and 2 is characterized in that: the add-on of the sodium hydroxide solution of 0.5mol/L is that every 100ml benzene and cadmium nitrate mixing solutions add 10mL.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408058A (en) * | 2013-08-22 | 2013-11-27 | 哈尔滨工程大学 | Room-temperature synthesis method of one-dimensional nano-zinc oxide with high gas-sensitive property |
| CN103482684A (en) * | 2013-09-23 | 2014-01-01 | 哈尔滨工程大学 | Preparation method for cadmium hydroxide nano-array capable of adsorbing and extracting DNA |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07161352A (en) * | 1993-12-08 | 1995-06-23 | Shin Kobe Electric Mach Co Ltd | Sintering cadmium negative electrode for alkaline storage battery |
| CN1139823A (en) * | 1995-04-11 | 1997-01-08 | 三洋电机株式会社 | High capacity long circulation time alkaline battery and making method of nickel electrode used for it |
| CN1546382A (en) * | 2003-12-10 | 2004-11-17 | 山东师范大学 | Method for synthesizing cadmium hydroxide single-crystal nanowire |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07161352A (en) * | 1993-12-08 | 1995-06-23 | Shin Kobe Electric Mach Co Ltd | Sintering cadmium negative electrode for alkaline storage battery |
| CN1139823A (en) * | 1995-04-11 | 1997-01-08 | 三洋电机株式会社 | High capacity long circulation time alkaline battery and making method of nickel electrode used for it |
| CN1546382A (en) * | 2003-12-10 | 2004-11-17 | 山东师范大学 | Method for synthesizing cadmium hydroxide single-crystal nanowire |
Non-Patent Citations (4)
| Title |
|---|
| 《Advanced Materials》 20080305 Vaishali R. Shinde et al. A Solution Chemistry Approach for the Selective Formation of Ultralong Nanowire Bundles of Crystalline Cd(OH)2 on Substrates 第1008至1012页 1-3 第20卷, 第5期 * |
| 《Applied Surface Science》 20090115 R.R. Salunkhe et al. Synthesis and characterization of cadmium hydroxide nano-nest by chemical route 第3924、3925页 1-3 第255卷, 第7期 * |
| R.R. SALUNKHE ET AL.: "Synthesis and characterization of cadmium hydroxide nano-nest by chemical route", 《APPLIED SURFACE SCIENCE》, vol. 255, no. 7, 15 January 2009 (2009-01-15), pages 3924 - 3925, XP025860579, DOI: doi:10.1016/j.apsusc.2008.10.035 * |
| VAISHALI R. SHINDE ET AL.: "A Solution Chemistry Approach for the Selective Formation of Ultralong Nanowire Bundles of Crystalline Cd(OH)2 on Substrates", 《ADVANCED MATERIALS》, vol. 20, no. 5, 5 March 2008 (2008-03-05), pages 1008 - 1012 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408058A (en) * | 2013-08-22 | 2013-11-27 | 哈尔滨工程大学 | Room-temperature synthesis method of one-dimensional nano-zinc oxide with high gas-sensitive property |
| CN103482684A (en) * | 2013-09-23 | 2014-01-01 | 哈尔滨工程大学 | Preparation method for cadmium hydroxide nano-array capable of adsorbing and extracting DNA |
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