CN105789601A - Preparation method of nanocluster divalent silver oxide positive electrode material - Google Patents
Preparation method of nanocluster divalent silver oxide positive electrode material Download PDFInfo
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- CN105789601A CN105789601A CN201410811926.9A CN201410811926A CN105789601A CN 105789601 A CN105789601 A CN 105789601A CN 201410811926 A CN201410811926 A CN 201410811926A CN 105789601 A CN105789601 A CN 105789601A
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Abstract
The invention relates to a preparation method of a nanocluster divalent silver oxide positive electrode material. The method comprises the following steps: pressing silver powder into silver plates; carrying out electrochemical pulse oxidation on the silver plates in an alkaline solution; and then washing and drying the silver plates, thereby finishing the preparation process of the nanocluster divalent silver oxide positive electrode material. By an electrochemical pulse oxidation method, the divalent silver oxide positive electrode material formed by clusters comprising silver oxide nanoparticles is prepared by adjusting the pulse frequency and controlling the growth morphology of the divalent silver oxide positive electrode material; the sizes of the nanoparticles are about 500nm; the sizes of the clusters are about 5 microns; and relatively large pores are formed between the clusters, so that ionic migration is facilitated; the size distribution is uniform; the product purity is high; the nanoclusters have multiple electrochemical active sites; the electrochemical activity is high; and the nanocluster divalent silver oxide positive electrode material has excellent discharge rate, very low electrode polarization and especially high electrochemical utilization rate, has excellent electrical properties, is simple in preparation process and does not contain other substance residues.
Description
Technical field
The invention belongs to electrokinetic cell positive electrode technical field, the preparation method particularly relating to a kind of nanocluster divalent silver oxide positive electrode.
Background technology
Divalent silver oxide (AgO) positive electrode has the stability of the high rate performance of excellence, higher specific capacity and brilliance, it is desirable thrust power cell positive material, is widely used in the military thrust power batteries such as aluminum silver battery, zinc-silver oxide cell and lithium silver battery.The pattern of divalent silver oxide positive electrode, purity directly affect its chemical property, and the chemical property of divalent silver oxide positive electrode is the deciding factor of above-mentioned electrokinetic cell performance.
Main deflection porous divalent silver oxide positive electrode and spininess divalent silver oxide positive electrode in the preparation of currently known divalent silver oxide positive electrode.Wherein porous divalent silver oxide positive electrode is generally first oxidized to common argentum powder monovalence silver oxide or divalent silver oxide positive electrode, then pass through electrochemical reducing and prepare macropore argentum powder, washing, dried macropore argentum powder tabletting, and constitute electrolysis bath with nickel sheet, alkaline solution carries out electrochemical oxidation, scrubbed, dry obtain porous divalent silver oxide positive electrode, the method only has certain effect in raising reactive ion migration velocity, during to electric discharge, faraday's reaction is then without helping, it is difficult to improve electrochemical properties；Spininess divalent silver oxide positive electrode generally adopts two-step method, first argentum powder is carried out in derivant derivant attachment, then argentum powder tabletted after an attachment, alkaline solution carries out electrochemical oxidation, scrubbed, dry obtain spininess divalent silver oxide positive electrode, the material electrochemical performance that the method is made is more excellent, but preparation process is more complicated, and has the residual of derivant.
Summary of the invention
The present invention solves the technical problem existed in known technology and provide that a kind of excellent electrical property, technique is simple, the preparation method of nanocluster divalent silver oxide positive electrode without other residues.
The present invention includes following technical scheme:
The preparation method of nanocluster divalent silver oxide positive electrode, is characterized in: include being pressed into argentum powder silver strip, after silver strip carries out electrochemistry pulse oxidizes in alkaline solution, washs, dries, namely completes the preparation process of nanocluster divalent silver oxide positive electrode.
The present invention can also adopt following technical measures:
Described silver strip is the argentum powder compacting after drying, sieving formed in vacuum drying oven；Described electrochemistry pulse oxidizes is: (1) selects the stainless steel substrates being slightly larger in dimension than silver strip size to be placed on the both sides of silver strip, silver strip and stainless steel substrates is placed in the lump in aqueous slkali；(2) silver strip is connected to the positive pole of pulse generator, and stainless steel substrates is connected to the negative pole of pulse generator, and the employing density of charging current is 8mA/cm2-4mA/cm2, discharge current density is 4mA/cm2-2mA/cm2, pulse frequency is 10Hz-50Hz, and electrochemical takes out after aoxidizing 20-32 hour；Described washing is wash the silver strip after electrochemistry pulse oxidizes to neutral with distilled water, described dries as vacuum drying；The nanocluster divalent silver oxide positive electrode made be nanocrystalline grain size length at 500 nanometers, cluster size is the multicrystal-state nano cluster divalent silver oxide positive electrode of 5 microns.
Described argentum powder is commercially available argentum powder.
Pulse generator used by described electrochemistry pulse oxidizes is direct current pulse power source.
Aqueous slkali used by described electrochemistry pulse oxidizes is sodium hydroxide solution, aqua calcis or potassium hydroxide solution.
The present invention has the advantage that and good effect:
1, the present invention adopts electrochemistry pulse oxidizes method, by regulating pulse frequency, control the growth morphology of divalent silver oxide positive electrode, prepare the divalent silver oxide positive electrode formed by the molecular cluster of silver oxide nanoparticle, wherein the size of nanoparticle is at 500 ran, the size of cluster is at 5 microns, there is between cluster and cluster bigger hole, it is easy to ion migration, even size distribution, product purity is high, nanocluster has more electro-chemical activity site, electro-chemical activity is high, there is the discharge-rate of excellence, low-down electrode polarization and extra high electrochemical utilization rate, there is the electrical property of excellence, and preparation process is simple, remain without other material.
2, the nanocluster divalent silver oxide positive electrode that the present invention makes is used in the batteries such as aluminum silver battery and zinc-silver oxide cell, has the discharge-rate of excellence, low-down electrode polarization and extra high electrochemical utilization rate, and battery has the electrical property of excellence.
Accompanying drawing explanation
Fig. 1 is nanocluster divalent silver oxide positive electrode x-ray diffraction pattern prepared by the present invention；
Fig. 2 is nanocluster divalent silver oxide positive electrode stereoscan photograph prepared by the present invention；
Fig. 3 is nanocluster divalent silver oxide positive electrode electrical property curve chart prepared by the present invention.
Detailed description of the invention
For the summary of the invention of the present invention, feature and effect can be disclosed further, describe in detail as follows especially exemplified by following instance.
The preparation method of nanocluster divalent silver oxide positive electrode, is characterized in: include being pressed into argentum powder silver strip, after silver strip carries out electrochemistry pulse oxidizes in alkaline solution, washs, dries, namely completes the preparation process of nanocluster divalent silver oxide positive electrode.
Described silver strip is the argentum powder compacting after drying, sieving formed in vacuum drying oven；Described electrochemistry pulse oxidizes is: (1) selects the stainless steel substrates being slightly larger in dimension than silver strip size to be placed on the both sides of silver strip, silver strip and stainless steel substrates is placed in the lump in aqueous slkali；(2) silver strip is connected to the positive pole of pulse generator, and stainless steel substrates is connected to the negative pole of pulse generator, and the employing density of charging current is 8mA/cm2-4mA/cm2, discharge current density is 4mA/cm2-2mA/cm2, pulse frequency is 10Hz-50Hz, and electrochemical takes out after aoxidizing 20-32 hour；Described washing is wash the silver strip after electrochemistry pulse oxidizes to neutral with distilled water, described dries as vacuum drying；The nanocluster divalent silver oxide positive electrode made be nanocrystalline grain size length at 500 nanometers, cluster size is the multicrystal-state nano cluster divalent silver oxide positive electrode of 5 microns.
Described argentum powder is commercially available argentum powder.
Pulse generator used by described electrochemistry pulse oxidizes is direct current pulse power source.
Aqueous slkali used by described electrochemistry pulse oxidizes is sodium hydroxide solution, aqua calcis or potassium hydroxide solution.
Embodiment 1:
Putting in vacuum drying oven by commercially available argentum powder, 60 DEG C dry 24 hours；Dried argentum powder tabletting, the size according to compacting silver strip, the stainless steel substrates selecting size bigger is placed on the both sides of silver strip, silver strip and stainless steel substrates is placed in the lump in sodium hydroxide solution；The silver strip wherein suppressed and the positive pole of direct current pulse power source connect, and the negative pole of stainless steel substrates and the pulse power connects, and adopt 8mA/cm2The density of charging current, 4mA/cm2Discharge current density, pulse frequency is 50Hz, and electrochemical oxidation took out after 20 hours, it is washed with distilled water to neutrality, 40 DEG C of vacuum dryings, after 12 hours, obtain nanocrystalline grain size length at 500 nanometers, and cluster size is the multicrystal-state nano cluster divalent silver oxide positive electrode of 5 microns.
Embodiment 2:
Putting in vacuum drying oven by commercially available argentum powder, 60 DEG C dry 24 hours；Dried argentum powder tabletting, the size according to compacting silver strip, the stainless steel substrates selecting size bigger is placed on the both sides of silver strip, silver strip and stainless steel substrates is placed in the lump in aqua calcis；The silver strip wherein suppressed and the positive pole of direct current pulse power source connect, and the negative pole of stainless steel substrates and DC source connects, and adopt 4mA/cm2The density of charging current, 2mA/cm2Discharge current density, pulse frequency is 30Hz, and electrochemical oxidation took out after 32 hours, it is washed with distilled water to neutrality, 60 DEG C of vacuum dryings, after 8 hours, obtain nanocrystalline grain size length at 500 nanometers, and cluster size is the multicrystal-state nano cluster divalent silver oxide positive electrode of 5 microns., after vacuum drying, obtain final products.In divalent silver oxide positive electrode nanocluster, nanocrystalline grain size length is at 500 ran, and cluster size is 5 microns.
Embodiment 3:
Putting in vacuum drying oven by commercially available argentum powder, 60 DEG C dry 24 hours.Dried argentum powder tabletting, the size according to compacting silver strip, the stainless steel substrates selecting size bigger is placed on the both sides of silver strip, silver strip and stainless steel substrates is placed in the lump in potassium hydroxide solution；The silver strip wherein suppressed and the positive pole of direct current pulse power source connect, and the negative pole of stainless steel substrates and DC source connects, and adopt 6mA/cm2The density of charging current, 3mA/cm2Discharge current density, pulse frequency is 10Hz, and electrochemical oxidation took out after 27 hours, it is washed with distilled water to neutrality, 30 DEG C of vacuum dryings, after 15 hours, obtain nanocrystalline grain size length at 500 nanometers, and cluster size is the multicrystal-state nano cluster divalent silver oxide positive electrode of 5 microns.
The nanocluster divalent silver oxide positive electrode embodiment of the present invention 1 prepared carries out X-ray diffraction test, microcosmic test and electrochemical properties test respectively, draws the stereoscan photograph shown in the x-ray diffraction pattern shown in Fig. 1, Fig. 2 and the electrical property curve chart shown in Fig. 3；As seen in Figure 1, the nanocluster divalent silver oxide positive electrode that prepared by the present invention has purity height, pollutant are few, adhesion good, mechanical strength is high, the feature of good environmental adaptability；As seen in Figure 2, the nanocluster divalent silver oxide positive electrode that prepared by the present invention is nanometer divalent silver oxide positive electrode crystal grain cluster of pattern rule on microcosmic；As seen in Figure 3, nanocluster divalent silver oxide positive electrode prepared by the present invention is that nanocrystal provides more faraday's avtive spot, shows the electrochemical properties of excellence, and material has good stability.
At electrolyte temperature 60-80 DEG C and 1C, the nanocluster divalent silver oxide positive electrode of the embodiment of the present invention 1 preparation is carried out below discharge-rate test, and result of the test is that (blanking voltage is not less than 1.40VVsAl/AlO for material effective2 -) specific energy is at more than 420mAh/g, electrochemical utilization rate is more than 95%, and average voltage is at 1.75V (VsAl/AlO2 -) more than.
The discharge-rate test that the nanocluster divalent silver oxide positive electrode of the embodiment of the present invention 2 preparation is carried out at electrolyte temperature 60-80 DEG C and 1C-5C, result of the test is that (blanking voltage is not less than 1.40VVsAl/AlO for material effective2 -) specific energy is at more than 400mAh/g, electrochemical utilization rate is more than 90%, and average voltage is at 1.60V (VsAl/AlO2 -) more than.
The discharge-rate test that the nanocluster divalent silver oxide positive electrode of the embodiment of the present invention 3 preparation is carried out at electrolyte temperature 60-80 DEG C and 5C, (blanking voltage is not less than 1.40VVsAl/AlO for this material effective2 -) specific energy is at more than 387mAh/g, electrochemical utilization rate is more than 85%, and average voltage is at 1.50V (VsAl/AlO2 -) more than.
Test result indicate that, nanocluster divalent silver oxide positive electrode prepared by the present invention has the discharge-rate of excellence, low-down electrode polarization and extra high electrochemical utilization rate.
The operation principle of the present invention:
The present invention adopts electrochemistry pulse oxidizes method, by regulating pulse frequency, control the growth morphology of divalent silver oxide positive electrode, prepare the divalent silver oxide positive electrode formed by the molecular cluster of silver oxide nanoparticle, wherein the size of nanoparticle is at 500 ran, the size of cluster is at 5 microns, there is between cluster and cluster bigger hole, it is easy to ion migration, even size distribution, product purity is high, and nanocluster has more electro-chemical activity site, electro-chemical activity is high, there is the discharge-rate of excellence, low-down electrode polarization and extra high electrochemical utilization rate.Not only preparation process is simple, remains without other material, and excellent electrical property.
Although above the preferred embodiments of the present invention being described; but the invention is not limited in above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is merely schematic; it is not restrictive; those of ordinary skill in the art is under the enlightenment of the present invention; without departing under present inventive concept and scope of the claimed protection situation, it is also possible to make a lot of form.These belong within protection scope of the present invention.
Claims (5)
1. the preparation method of nanocluster divalent silver oxide positive electrode, it is characterized in that: include argentum powder is pressed into silver strip, after silver strip carries out electrochemistry pulse oxidizes in alkaline solution, wash, dry, namely complete the preparation process of nanocluster divalent silver oxide positive electrode.
2. the preparation method of nanocluster divalent silver oxide positive electrode according to claim 1, it is characterised in that: described silver strip is the argentum powder compacting after drying, sieving formed in vacuum drying oven；Described electrochemistry pulse oxidizes is: (1) selects the stainless steel substrates being slightly larger in dimension than silver strip size to be placed on the both sides of silver strip, silver strip and stainless steel substrates is placed in the lump in aqueous slkali；(2) silver strip is connected to the positive pole of pulse generator, and stainless steel substrates is connected to the negative pole of pulse generator, and the employing density of charging current is 8mA/cm2-4mA/cm2, discharge current density is 4mA/cm2-2mA/cm2, pulse frequency is 10Hz-50Hz, and electrochemical takes out after aoxidizing 20-32 hour；Described washing is wash the silver strip after electrochemistry pulse oxidizes to neutral with distilled water, described dries as vacuum drying；The nanocluster divalent silver oxide positive electrode made be nanocrystalline grain size length at 500 nanometers, cluster size is the multicrystal-state nano cluster divalent silver oxide positive electrode of 5 microns.
3. the preparation method of nanocluster divalent silver oxide positive electrode according to claim 1 or claim 2, it is characterised in that: described argentum powder is commercially available argentum powder.
4. the preparation method of nanocluster divalent silver oxide positive electrode according to claim 1 or claim 2, it is characterised in that: the pulse generator used by described electrochemistry pulse oxidizes is direct current pulse power source.
5. the preparation method of nanocluster divalent silver oxide positive electrode according to claim 1 or claim 2, it is characterised in that: the aqueous slkali used by described electrochemistry pulse oxidizes is sodium hydroxide solution, aqua calcis or potassium hydroxide solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113871738A (en) * | 2021-09-24 | 2021-12-31 | 贵州梅岭电源有限公司 | Electrode charging method for improving capacity of zinc-silver reserve battery |
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| JPS59182228A (en) * | 1983-03-31 | 1984-10-17 | Mitsui Mining & Smelting Co Ltd | Silver (ii) peroxide and cell using the same |
| CN1929169A (en) * | 2006-09-25 | 2007-03-14 | 梅岭化工厂 | Method for making thin type silver electrode of silver-zinc battery |
| CN102945957A (en) * | 2012-12-07 | 2013-02-27 | 中国电子科技集团公司第十八研究所 | Preparation method of spiny silver peroxide anode material |
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- 2014-12-22 CN CN201410811926.9A patent/CN105789601A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59182228A (en) * | 1983-03-31 | 1984-10-17 | Mitsui Mining & Smelting Co Ltd | Silver (ii) peroxide and cell using the same |
| CN1929169A (en) * | 2006-09-25 | 2007-03-14 | 梅岭化工厂 | Method for making thin type silver electrode of silver-zinc battery |
| CN102945957A (en) * | 2012-12-07 | 2013-02-27 | 中国电子科技集团公司第十八研究所 | Preparation method of spiny silver peroxide anode material |
Non-Patent Citations (1)
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| 曾华粱，杨家昌: "《电解和化学转化膜》", 30 April 1987, 轻工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113871738A (en) * | 2021-09-24 | 2021-12-31 | 贵州梅岭电源有限公司 | Electrode charging method for improving capacity of zinc-silver reserve battery |
| CN113871738B (en) * | 2021-09-24 | 2023-09-26 | 贵州梅岭电源有限公司 | Electrode charging method for improving capacity of zinc-silver reserve battery |
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Application publication date: 20160720 |