CN102522139A - 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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- CN102522139A CN102522139A CN2011103369103A CN201110336910A CN102522139A CN 102522139 A CN102522139 A CN 102522139A CN 2011103369103 A CN2011103369103 A CN 2011103369103A CN 201110336910 A CN201110336910 A CN 201110336910A CN 102522139 A CN102522139 A CN 102522139A
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- iridium
- hydrous oxide
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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 the part transition metal oxide has the characteristic that discharges and recharges of similar electric capacity; People begin metal oxide materials is given the attention of height; Proposed respectively to can be used for preparing candidate's oxide material of electrode material for super capacitor gradually, wherein outstanding with the ruthenium-oxide of hydration 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 oxide film material that has the hydration structure in the matrix surface preparation through the mode of electroplating; This method has advantage simple to operate; But electrodeposition process requires a large amount of electrolyte; And the metal ion in the electrolyte can not make full use of, and has the waste of raw materials important disadvantages; Sol-gal process, chemical precipitation method, hydro thermal method etc. can prepare the oxide powder material of hydration structure, but these preparation methods require comparatively harsh, slight condition variation possibly 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 have very high ratio electric capacity and cycle charge discharge electrical stability directly as the electrode material of ultracapacitor, is the ideal electrode material of preparation high-performance ultracapacitor.In addition, preparation method provided by the invention has advantages such as technology is simple, the cycle is short, cost is low, can repeat, and can be used as the suitability for industrialized production technology and uses.
For reaching above-mentioned purpose, 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 the said cobalt iridium hydrous oxide: the Ir mol ratio is 20～80: 80～20, and the preparation method of this cobalt iridium hydrous oxide comprises the steps:
1) with crystallization cobalt chloride (CoCl
26H
2O), chloro-iridic acid (H
2IrCl
6) to be dissolved into volume ratio be in 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 the enamel crucible; Hold one glass of clear water with the enamel crucible in addition; Two crucibles are placed box type furnace in the lump, closed behind the fire door insulation 1 to 2 hour, holding temperature is set in 300～400 ℃; With the stove cooling, promptly obtain cobalt iridium hydrous oxide material then.
A kind of said cobalt iridium hydrous oxide film is made up of cobalt iridium hydrous oxide and conductive agent by the formed cobalt iridium of cobalt iridium hydrous oxide hydrous oxide film, and wherein conductive agent accounts for 5～10% of cobalt iridium hydrous oxide film gross mass.
A kind of method for preparing cobalt iridium hydrous oxide film comprises the steps:
1) with crystallization cobalt chloride (CoCl
26H
2O), chloro-iridic acid (H
2IrCl
6) to be dissolved into volume ratio be in 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 the enamel crucible; Hold one glass of clear water with the enamel crucible in addition; Two crucibles are placed box type furnace in the lump, closed behind the fire door insulation 1 to 2 hour, holding temperature is set in 300～400 ℃; With the stove cooling, promptly obtain cobalt iridium hydrous oxide material then;
3) with step 2) the cobalt iridium hydrous oxide material that makes and conductive agent, adhesive (ptfe emulsion) be 95～90: 5～10 by weight proportion: 5～15 mix, and are modulated into pastel;
4) pastel is coated in the conducting base surface equably; Be pressed into behind the pole piece under 200～280 ℃ of temperature heat treatment 30-60 minute with powder compressing machine then; Purpose 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 a in carbon black, carbon fiber, the carbosphere.
Adhesive adopts ptfe emulsion in the said step 3).
Conducting base is any one in titanium, tantalum, nickel, the aluminium in the said step 4).
The effect of the clear water step 2) provides high-temperature water vapor; In box type furnace; Water in the crucible is because of the hot environment rapid evaporation, makes to be full of high-temperature steam, metal chloride decomposes and oxidized in the burner hearth; And combine, thereby formed the oxide of hydration structure with high-temperature steam in the burner hearth.
The invention has the beneficial effects as follows: the thin-film material that the cobalt iridium oxide of hydration structure provided by the invention forms can be directly as the electrode material of ultracapacitor; Characteristic with high specific capacitance, high stability, be preparation high-performance ultracapacitor than good material.And preparation method of the present invention has, and technology is simple, cost is low, the cycle is short, can repeat, the characteristics of suitable 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 merely preferred embodiment of the present invention, and all equivalent variations and modifications of doing according to claim of the present invention 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: the Ir mol ratio is 20: 80.The preparation process of this cobalt iridium hydrous oxide is following:
1) with 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 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 the enamel crucible; Hold one glass of clear water with the enamel crucible in addition; Two crucibles are placed box type furnace in the lump, closed behind the fire door insulation 2 hours, respectively 300 ℃, 350 ℃, 400 ℃ insulations; The cooling of coming out of the stove, promptly obtain Co: the Ir mol ratio is 20: 80 a cobalt iridium hydrous oxide material.
A kind of by the formed cobalt iridium of above-mentioned cobalt iridium hydrous oxide hydrous oxide film; Said 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 said conductive agent is a carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film comprises the steps:
1) with 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 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 the enamel crucible; Hold one glass of clear water with the enamel crucible in addition; Two crucibles are placed box type furnace in the lump, closed behind the fire door insulation 2 hours, respectively 300 ℃, 350 ℃, 400 ℃ insulations; The cooling of coming out of the stove, promptly obtain Co: the Ir mol ratio is 20: 80 a cobalt iridium hydrous oxide material;
3) with step 2) the cobalt iridium hydrous oxide material that makes and carbon black (conductive agent), ptfe emulsion (adhesive) be to mix at 90: 10: 15 in proportion, is modulated into pastel;
4) pastel is coated in titanium conducting base surface equably; Be pressed into behind the pole piece under 220 ℃ of temperature heat treatment 45 minutes with powder compressing machine; Purpose 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: the Ir mol ratio is 40: 60.The preparation process of this cobalt iridium hydrous oxide is following:
1) with 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 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 the enamel crucible; Hold one glass of clear water with the enamel crucible in addition, two crucibles are placed box type furnace in the lump, close behind the fire door 350 ℃ of insulations 1.5 hours; The cooling of coming out of the stove, promptly obtain Co: the Ir mol ratio is 40: 60 a cobalt iridium hydrous oxide material;
A kind of by the formed cobalt iridium of above-mentioned cobalt iridium hydrous oxide hydrous oxide film; Said 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 said conductive agent is a carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film comprises the steps:
1) with 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 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 the enamel crucible, holds one glass of clear water with the enamel crucible in addition, two crucibles are placed box type furnace in the lump, close behind the fire door 350 ℃ of insulations 1.5 hours, the cooling of coming out of the stove promptly obtains cobalt iridium hydrous oxide material;
3) with step 2) the cobalt iridium hydrous oxide material that makes and carbon black (conductive agent), ptfe emulsion (adhesive) be to mix at 95: 5: 15 in proportion, and add an amount of absolute ethyl alcohol, be modulated into pastel;
4) pastel is coated in tantalum conducting base surface equably; Be pressed into behind the pole piece under 240 ℃ of temperature heat treatment 30 minutes with powder compressing machine; Purpose 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: the Ir mol ratio is 60: 40.The preparation process of this cobalt iridium hydrous oxide is following:
1) with 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 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 the enamel crucible, holds one glass of clear water with the enamel crucible in addition, two crucibles are placed box type furnace in the lump, close behind the fire door 350 ℃ of insulations 1 hour, the cooling of coming out of the stove promptly obtains cobalt iridium hydrous oxide material.
A kind of by the formed cobalt iridium of above-mentioned cobalt iridium hydrous oxide hydrous oxide film; Said 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 said conductive agent is a carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film comprises the steps:
1) with 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 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 the enamel crucible, holds one glass of clear water with the enamel crucible in addition, two crucibles are placed box type furnace in the lump, close behind the fire door 350 ℃ of insulations 1 hour, the cooling of coming out of the stove promptly obtains cobalt iridium hydrous oxide material;
3) with step 2) the cobalt iridium hydrous oxide material that makes and carbosphere (conductive agent), ptfe emulsion (adhesive) be to mix at 95: 5: 10 in proportion, and add an amount of absolute ethyl alcohol, be modulated into pastel;
4) pastel is coated in nickel conducting base surface equably; Be pressed into behind the pole piece under 200 ℃ of temperature heat treatment 60 minutes with powder compressing machine; Purpose 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: the Ir mol ratio is 80: 20.The preparation process of this cobalt iridium hydrous oxide is following:
1) with 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 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 the enamel crucible; Hold one glass of clear water with the enamel crucible in addition, two crucibles are placed box type furnace in the lump, close behind the fire door 350 ℃ of insulations 1 hour; The cooling of coming out of the stove, promptly obtain Co: the Ir mol ratio is 80: 20 a cobalt iridium hydrous oxide material.
A kind of by the formed cobalt iridium of above-mentioned cobalt iridium hydrous oxide hydrous oxide film; Said 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 said conductive agent is a carbon black.
The preparation method of above-mentioned cobalt iridium hydrous oxide film comprises the steps:
1) with 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 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 the enamel crucible, holds one glass of clear water with the enamel crucible in addition, two crucibles are placed box type furnace in the lump, close behind the fire door 350 ℃ of insulations 1 hour, the cooling of coming out of the stove promptly obtains cobalt iridium hydrous oxide material;
3) with step 2) the cobalt iridium hydrous oxide material that makes and carbon fiber (conductive agent), ptfe emulsion (adhesive) be to mix at 90: 10: 5 in proportion, and add an amount of absolute ethyl alcohol, be modulated into pastel;
4) pastel is coated in aluminium conducting base surface equably; Be pressed into behind the pole piece under 260 ℃ of temperature heat treatment 40 minutes with powder compressing machine; Purpose 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 the iridium cobalt hydrous oxide of each enforcement preparation adopts the anti-company of speeding of Germany to produce is tested, and the result is organized in the table 1, and table 1 is each embodiment experimental test result.The prepared film material can directly use as electrode material among the embodiment 1 to 4.Employing standard three-electrode system adopts Shanghai occasion China CHI660C electrochemical workstation can measure the capacitive property of the thin-film material of each embodiment preparation, and the result is organized in the table 1.The experiment proof; Each item chemical property of cobalt iridium hydrous oxide film is good; Reach as high as 587.63F/g than electric capacity; Experience discharge and recharge for 10,000 times after, the electric capacity conservation rate proves fully that all more than 94% cobalt iridium hydrous oxide film provided by the invention is the preferred electrode materials of the high-quality electrochemical capacitor of preparation.
Table 1
Claims (6)
1. cobalt iridium hydrous oxide, it is characterized in that: said 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 the said cobalt iridium hydrous oxide: the Ir mol ratio is 20～80: 80～20; The first-selected crystallization cobalt chloride (CoCl that adopts
26H
2O), chloro-iridic acid (H
2IrCl
6) be raw material, be dissolved into volume ratio and be in ethanol-isopropyl alcohol mixed solvent of 2: 1, make cobalt iridium chloride precursor solution; Then cobalt iridium chloride precursor solution is contained up in the enamel crucible; Hold one glass of clear water with the enamel crucible in addition; Two crucibles are placed box type furnace in the lump, closed behind the fire door insulation 1 to 2 hour, holding temperature is set in 300～400 ℃; With the stove cooling, promptly obtain cobalt iridium hydrous oxide material then.
2. the formed cobalt iridium of cobalt iridium hydrous oxide as claimed in claim 1 hydrous oxide film; It is characterized in that: said 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.
3. method for preparing cobalt iridium hydrous oxide film as claimed in claim 2, it is characterized in that: this method comprises the steps:
1) with crystallization cobalt chloride (CoCl
26H
2O), chloro-iridic acid (H
2IrCl
6) to be dissolved into volume ratio be in 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 the enamel crucible; Hold one glass of clear water with the enamel crucible in addition; Two crucibles are placed box type furnace in the lump, closed behind the fire door insulation 1 to 2 hour, holding temperature is set in 300～400 ℃; With the stove cooling, promptly obtain cobalt iridium hydrous oxide material then;
3) with step 2) the cobalt iridium hydrous oxide material that makes and conductive agent, adhesive be 95～90: 5～10 by weight proportion: 5～15 mix, and are modulated into pastel;
4) pastel is coated in the conducting base surface equably; Be pressed into behind the pole piece under 200～280 ℃ of temperature heat treatment 30-60 minute with powder compressing machine then; Purpose 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.
4. cobalt iridium hydrous oxide film according to claim 3 is characterized in that: conductive agent is at least a in carbon black, carbon fiber, the carbosphere in the said step 3).
5. cobalt iridium hydrous oxide film according to claim 3 is characterized in that: adhesive adopts ptfe emulsion in the said step 3).
6. the method for preparing cobalt iridium hydrous oxide film according to claim 3 is characterized in that: the conducting base in the said step 4) is any one in titanium, tantalum, nickel, the aluminium.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004303678A (en) * | 2003-04-01 | 2004-10-28 | Hitachi Maxell Ltd | Energy storage element and combined energy storage element |
| CN101290835A (en) * | 2007-04-16 | 2008-10-22 | 韩国科学技术研究院 | Electrode for supercapacitor and the fabrication method thereof |
| CN102169759A (en) * | 2010-12-17 | 2011-08-31 | 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 |
-
2011
- 2011-10-28 CN CN201110336910.3A patent/CN102522139B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004303678A (en) * | 2003-04-01 | 2004-10-28 | Hitachi Maxell Ltd | Energy storage element and combined energy storage element |
| CN101290835A (en) * | 2007-04-16 | 2008-10-22 | 韩国科学技术研究院 | Electrode for supercapacitor and the fabrication method thereof |
| CN102169759A (en) * | 2010-12-17 | 2011-08-31 | 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 |
Non-Patent Citations (1)
| Title |
|---|
| A. A. F. GRUPIONI等: "Effect of the Co3O4 Introduction in the Pseudocapacitive Behavior of IrO2-Based Electrode", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 * |
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