CN102522139B - Cobalt iridium hydrous oxide, cobalt iridium hydrous oxide film and film preparation method - Google Patents
Cobalt iridium hydrous oxide, cobalt iridium hydrous oxide film and film preparation method Download PDFInfo
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- CN102522139B CN102522139B CN201110336910.3A CN201110336910A CN102522139B CN 102522139 B CN102522139 B CN 102522139B CN 201110336910 A CN201110336910 A CN 201110336910A CN 102522139 B CN102522139 B CN 102522139B
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- cobalt
- iridium
- hydrous oxide
- cobalt iridium
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Abstract
The invention discloses a cobalt iridium hydrous oxide. The cobalt iridium hydrous oxide is composed of hydrous iridium oxide and hydrous cobalt oxide and is expressed as: (Co3O4+IrO2).xH2O, wherein the x is 0.3 to 2. And in the cobalt iridium hydrous oxide, a molar ratio of Co to Ir is 20 - 80 : 80 - 20. besides, the preparation method of a cobalt iridium hydrous oxide film comprises the following steps that: (1), crystallized cobaltous chloride and chloro-iridic acid are dissolved into a ethanol-isopropanol mixed solvent with a volume ratio of the ethanol to the isopropanol being 2 to 1, so that a cobalt iridium chloride precursor solution is prepared; and (2), the cobalt iridium chloride precursor solution is held and placed into an enamel crucible and another enamel crucible is used to carry a cup of clear water; the two crucibles are placed in a box-type furnace, and after the furnace is closed, the temperature is preserved for 1 to 2 hours, wherein the temperature is set at a range from 300 DEGC to 400 DEG C; and then cooling in furnace is carried out, so that a cobalt iridium hydrous oxide material is obtained. According to the invention, a film material that is prepared by cobalt iridium oxide with a hydrous structure is an ideal material for preparing a super capacitor; and the preparation method is simple and can be applied as an industrialized production technology.
Description
Technical field
The present invention relates to a kind of cobalt iridium hydrous oxide, cobalt iridium hydrous oxide film, and method for manufacturing thin film.
Background technology
Nineteen fifty-seven Beeker finds to adopt the material with carbon element of high-ratio surface can prepare a kind of novel capacitor with high ratio electric capacity, specific power and high rate during charging-discharging.The energy storage mechanism of this capacitor is at electrode and electrolyte interface stored charge, forms the storage of electric double layer electric weight, is referred to as " double electric layer capacitor " or " ultracapacitor " by people.Subsequently, B.E.Conway finds that part transition metal oxide has the feature that discharges and recharges of similar electric capacity, people start metal oxide materials to give the attention of height, propose gradually respectively to can be used for preparing candidate's oxide material of electrode material for super capacitor, wherein outstanding with the ruthenium-oxide of Hydrated structure and yttrium oxide and the performance of their composite material.At present, the method for preparing hydrous oxide comprises: electrochemical deposition method, sol-gal process, chemical precipitation method and hydro thermal method.Electrochemical deposition method is the mode by electroplating has Hydrated structure oxide film material in matrix surface preparation, this method has advantages of simple to operate, but electrodeposition process requires a large amount of electrolyte, and the metal ion in electrolyte can not make full use of, there is the shortcoming that waste of raw materials is serious; Sol-gal process, chemical precipitation method, hydro thermal method etc. can be prepared the oxide powder material of Hydrated structure, but these preparation methods require comparatively harsh, slight condition variation may cause the structure of product to change a lot to process conditions, and poor repeatability.
Summary of the invention
The object of the present invention is to provide a kind of cobalt iridium hydrous oxide, cobalt iridium hydrous oxide thin-film material, and thin-film material preparation method; Cobalt iridium hydrous oxide thin-film material provided by the invention can, directly as the electrode material of ultracapacitor, have very high ratio electric capacity and cycle charge discharge electrical stability, is the ideal electrode material of preparing high-performance super capacitor.In addition, preparation method provided by the invention has the advantages such as technique is simple, the cycle is short, cost is low, can repeat, and can be used as Industrialized processing technique and uses.
For reaching above-mentioned object, the present invention adopts following technical scheme:
A kind of cobalt iridium hydrous oxide, is made up of aqua oxidation iridium and aqua oxidation cobalt, is expressed as: (Co
3o
4+ IrO
2) xH
2o, wherein x is 0.3～2; Co in described cobalt iridium hydrous oxide: Ir mol ratio is 20～80: 80～20, the preparation method of this cobalt iridium hydrous oxide comprises the steps:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) to be dissolved into volume ratio be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, after closing fire door, be incubated 1 to 2 hour, holding temperature is set in 300～400 DEG C, then cooling with stove, obtain cobalt iridium hydrous oxide material.
The cobalt iridium hydrous oxide film being formed by cobalt iridium hydrous oxide, described cobalt iridium hydrous oxide film is made up of cobalt iridium hydrous oxide and conductive agent, and wherein conductive agent accounts for 5～10% of cobalt iridium hydrous oxide film gross mass.
A method of preparing cobalt iridium hydrous oxide film, comprises the steps:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) to be dissolved into volume ratio be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, after closing fire door, be incubated 1 to 2 hour, holding temperature is set in 300～400 DEG C, then cooling with stove, obtain cobalt iridium hydrous oxide material;
3) by step 2) the cobalt iridium hydrous oxide material that makes is 95～90: 5～10 with conductive agent, adhesive (ptfe emulsion) by weight proportion: 5～15 mix, and are modulated into pastel;
4) pastel is coated in to conducting base surface equably, then be pressed into after pole piece heat treatment 30-60 minute at 200～280 DEG C of temperature with powder compressing machine, object is to make the oxidized decomposition of adhesive, thereby makes the cobalt iridium hydrous oxide thin-film material of cobalt iridium hydrous oxide and conductive agent formation.
Described step 3) conductive agent is at least one in carbon black, carbon fiber, carbosphere.
Described step 3) middle adhesive employing ptfe emulsion.
Described step 4) in conducting base be any one in titanium, tantalum, nickel, aluminium.
Step 2) described in the effect of clear water be to provide high-temperature water vapor, in box type furnace, water in crucible is because of hot environment rapid evaporation, make to be full of in burner hearth high-temperature steam, metal chloride decomposes and oxidized, and high-temperature steam in burner hearth is combined, thereby form the oxide of Hydrated structure.
The invention has the beneficial effects as follows: the thin-film material that the cobalt iridium oxide of Hydrated structure provided by the invention forms can be directly as the electrode material of ultracapacitor, there is the characteristic of high specific capacitance, high stability, be prepare high-performance super capacitor compared with good material.And preparation method of the present invention has, and technique is simple, cost is low, the cycle is short, can repeat, the feature of the applicable suitability for industrialized production such as workable.Application of the present invention has positive effect to the development that promotes material preparation technology and electrical power storage technology.
Embodiment
The following stated is only preferred embodiment of the present invention, and all equivalent variations of doing according to the present patent application the scope of the claims and modification all should belong to covering scope of the present invention.
Embodiment 1
A kind of cobalt iridium hydrous oxide, is made up of aqua oxidation iridium and aqua oxidation cobalt, is expressed as: (Co
3o
4+ IrO
2) xH
2o, Co: Ir mol ratio is 20: 80.The preparation process of this cobalt iridium hydrous oxide is as follows:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 20: 80 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, after closing fire door, be incubated 2 hours, respectively 300 DEG C, 350 DEG C, 400 DEG C insulations, come out of the stove cooling, obtain Co: the cobalt iridium hydrous oxide material that Ir mol ratio is 20: 80.
A kind of cobalt iridium hydrous oxide film being formed by above-mentioned cobalt iridium hydrous oxide, described cobalt iridium hydrous oxide thin-film material is made up of cobalt iridium hydrous oxide and conductive agent, wherein conductive agent accounts for 10% of cobalt iridium hydrous oxide film gross mass, and described conductive agent is carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film, comprises the steps:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 20: 80 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, after closing fire door, be incubated 2 hours, respectively 300 DEG C, 350 DEG C, 400 DEG C insulations, come out of the stove cooling, obtain Co: the cobalt iridium hydrous oxide material that Ir mol ratio is 20: 80;
3) by step 2) the cobalt iridium hydrous oxide material that makes is to mix at 90: 10: 15 with carbon black (conductive agent), ptfe emulsion (adhesive) in proportion, is modulated into pastel;
4) pastel is coated in equably to titanium conducting base surface, be pressed into after pole piece at 220 DEG C of temperature heat treatment 45 minutes with powder compressing machine, object is to make the oxidized decomposition of adhesive, thereby makes the cobalt iridium hydrous oxide thin-film material of cobalt iridium hydrous oxide and conductive agent formation.
Embodiment 2
A kind of cobalt iridium hydrous oxide, is made up of aqua oxidation iridium and aqua oxidation cobalt, is expressed as: (Co
3o
4+ IrO
2) xH
2o, Co: Ir mol ratio is 40: 60.The preparation process of this cobalt iridium hydrous oxide is as follows:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 40: 60 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, after closing fire door, be incubated 1.5 hours at 350 DEG C, come out of the stove cooling, obtain Co: the cobalt iridium hydrous oxide material that Ir mol ratio is 40: 60;
A kind of cobalt iridium hydrous oxide film being formed by above-mentioned cobalt iridium hydrous oxide, described cobalt iridium hydrous oxide thin-film material is made up of cobalt iridium hydrous oxide and conductive agent, wherein conductive agent accounts for 5% of cobalt iridium hydrous oxide film gross mass, and described conductive agent is carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film, comprises the steps:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 40: 60 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, close after fire door 350 DEG C of insulations 1.5 hours, come out of the stove cooling, obtain cobalt iridium hydrous oxide material;
3) by step 2) the cobalt iridium hydrous oxide material that makes is to mix at 95: 5: 15 with carbon black (conductive agent), ptfe emulsion (adhesive) in proportion, and add appropriate absolute ethyl alcohol, be modulated into pastel;
4) pastel is coated in equably to tantalum conducting base surface, be pressed into after pole piece at 240 DEG C of temperature heat treatment 30 minutes with powder compressing machine, object is to make the oxidized decomposition of adhesive, thereby makes the cobalt iridium hydrous oxide thin-film material of cobalt iridium hydrous oxide and conductive agent formation.
Embodiment 3
A kind of cobalt iridium hydrous oxide, is made up of aqua oxidation iridium and aqua oxidation cobalt, is expressed as: (Co
3o
4+ IrO
2) xH
2o, Co: Ir mol ratio is 60: 40.The preparation process of this cobalt iridium hydrous oxide is as follows:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 60: 40 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, holds one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, close after fire door 350 DEG C of insulations 1 hour, come out of the stove cooling, obtain cobalt iridium hydrous oxide material.
A kind of cobalt iridium hydrous oxide film being formed by above-mentioned cobalt iridium hydrous oxide, described cobalt iridium hydrous oxide thin-film material is made up of cobalt iridium hydrous oxide and conductive agent, wherein conductive agent accounts for 5% of cobalt iridium hydrous oxide film gross mass, and described conductive agent is carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film, comprises the steps:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 60: 40 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, holds one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, close after fire door 350 DEG C of insulations 1 hour, come out of the stove cooling, obtain cobalt iridium hydrous oxide material;
3) by step 2) the cobalt iridium hydrous oxide material that makes is to mix at 95: 5: 10 with carbosphere (conductive agent), ptfe emulsion (adhesive) in proportion, and add appropriate absolute ethyl alcohol, be modulated into pastel;
4) pastel is coated in equably to nickel conducting base surface, be pressed into after pole piece at 200 DEG C of temperature heat treatment 60 minutes with powder compressing machine, object is to make the oxidized decomposition of adhesive, thereby makes the cobalt iridium hydrous oxide thin-film material of cobalt iridium hydrous oxide and conductive agent formation.
Embodiment 4
A kind of cobalt iridium hydrous oxide, is made up of aqua oxidation iridium and aqua oxidation cobalt, is expressed as: (Co
3o
4+ IrO
2) xH
2o, Co: Ir mol ratio is 80: 20.The preparation process of this cobalt iridium hydrous oxide is as follows:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 80: 20 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, close after fire door 350 DEG C of insulations 1 hour, come out of the stove cooling, obtain Co: the cobalt iridium hydrous oxide material that Ir mol ratio is 80: 20.
A kind of cobalt iridium hydrous oxide film being formed by above-mentioned cobalt iridium hydrous oxide, described cobalt iridium hydrous oxide thin-film material is made up of cobalt iridium hydrous oxide and conductive agent, wherein conductive agent accounts for 10% of cobalt iridium hydrous oxide film gross mass, and described conductive agent is carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film, comprises the steps:
1) by crystallization cobalt chloride (CoCl
26H
2o), chloro-iridic acid (H
2irCl
6) be that to be dissolved into volume ratio at 80: 20 be, in the ethanol-isopropyl alcohol mixed solvent of 2: 1, to make cobalt iridium chloride precursor solution in molar ratio;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, holds one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, close after fire door 350 DEG C of insulations 1 hour, come out of the stove cooling, obtain cobalt iridium hydrous oxide material;
3) by step 2) the cobalt iridium hydrous oxide material that makes is to mix at 90: 10: 5 with carbon fiber (conductive agent), ptfe emulsion (adhesive) in proportion, and add appropriate absolute ethyl alcohol, be modulated into pastel;
4) pastel is coated in equably to aluminium conducting base surface, be pressed into after pole piece at 260 DEG C of temperature heat treatment 40 minutes with powder compressing machine, object is to make the oxidized decomposition of adhesive, thereby makes the cobalt iridium hydrous oxide thin-film material of cobalt iridium hydrous oxide and conductive agent formation.
The thermogravimetric analyzer that the water content of each iridium cobalt hydrous oxide of implementing preparation adopts German Nai Chi company to produce is tested, and result is organized in table 1, and table 1 is each embodiment experimental test result.Thin-film material prepared in embodiment 1 to 4 can directly use as electrode material.Employing standard three-electrode system, adopts Shanghai occasion China CHI660C electrochemical workstation can measure the capacitive property of thin-film material prepared by each embodiment, and result is organized in table 1.Experimental results show that, every chemical property of cobalt iridium hydrous oxide film is good, reach as high as 587.63F/g than electric capacity, after experiencing and discharging and recharging for 10,000 times, electric capacity conservation rate all, more than 94%, fully proves that cobalt iridium hydrous oxide film provided by the invention is the preferred electrode materials of preparation high-quality electrochemical capacitor.
Table 1
Claims (1)
1. a method of preparing cobalt iridium hydrous oxide film, is characterized in that: the method comprises the steps:
1) crystallization cobalt chloride, chloro-iridic acid are dissolved in ethanol-isopropyl alcohol mixed solvent that volume ratio is 2:1, make cobalt iridium chloride precursor solution;
2) cobalt iridium chloride precursor solution is contained up in enamel crucible, hold one glass of clear water with enamel crucible in addition, two crucibles are placed in to box type furnace in the lump, after closing fire door, be incubated 1 to 2 hour, holding temperature is set in 300～400 DEG C, then cooling with stove, obtain cobalt iridium hydrous oxide material; Described cobalt iridium hydrous oxide is made up of aqua oxidation iridium and aqua oxidation cobalt, is expressed as: (Co
3o
4+ IrO
2) xH
2o, wherein x is 0.3～2; Co in described cobalt iridium hydrous oxide: Ir mol ratio is 20～80: 80～20;
3) by step 2) the cobalt iridium hydrous oxide material that makes is 95～90: 5～10 with conductive agent, adhesive by weight proportion: 5～15 mix, and are modulated into pastel;
4) pastel is coated in to conducting base surface equably, then be pressed into after pole piece heat treatment 30-60 minute at 200～280 DEG C of temperature with powder compressing machine, object is to make the oxidized decomposition of adhesive, thereby makes the cobalt iridium hydrous oxide thin-film material of cobalt iridium hydrous oxide and conductive agent formation; Described cobalt iridium hydrous oxide film is made up of cobalt iridium hydrous oxide and conductive agent, and wherein conductive agent accounts for 5～10% of cobalt iridium hydrous oxide film gross mass;
Described step 3) in conductive agent be at least one in carbon black, carbon fiber, carbosphere;
Described step 3) middle adhesive employing ptfe emulsion;
Described step 4) in conducting base be any one in titanium, tantalum, nickel, aluminium.
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| CN201110336910.3A CN102522139B (en) | 2011-10-28 | 2011-10-28 | Cobalt iridium hydrous oxide, cobalt iridium hydrous oxide film and film preparation method |
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| JP2004303678A (en) * | 2003-04-01 | 2004-10-28 | Hitachi Maxell Ltd | Energy storage element and combined energy storage element |
| KR100894481B1 (en) * | 2007-04-16 | 2009-04-22 | 한국과학기술연구원 | Electrode for supercapacitor having metal oxide deposited onto ultrafine carbon fiber and the fabrication method thereof |
| CN102169759B (en) * | 2010-12-17 | 2013-04-17 | 中国振华（集团）新云电子元器件有限责任公司 | Preparation method of ruthenium oxide electrode material |
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Non-Patent Citations (2)
| Title |
|---|
| A. A. F. Grupioni等.Effect of the Co3O4 Introduction in the Pseudocapacitive Behavior of IrO2-Based Electrode.《Journal of The Electrochemical Society》.2001,第148卷(第9期),A1015-A1022. * |
| Effect of the Co3O4 Introduction in the Pseudocapacitive Behavior of IrO2-Based Electrode;A. A. F. Grupioni等;《Journal of The Electrochemical Society》;20010810;第148卷(第9期);A1015-A1022 * |
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