CN102168283A - Electrode coating and preparation method thereof - Google Patents
Electrode coating and preparation method thereof Download PDFInfo
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- CN102168283A CN102168283A CN2011100879195A CN201110087919A CN102168283A CN 102168283 A CN102168283 A CN 102168283A CN 2011100879195 A CN2011100879195 A CN 2011100879195A CN 201110087919 A CN201110087919 A CN 201110087919A CN 102168283 A CN102168283 A CN 102168283A
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Abstract
The invention discloses a high-adhesiveness durable electrode coating and a preparation method thereof. The electrode coating is prepared by adding a coordination compound into an iridium-tantalum coating, wherein the coordinator is one, two or three of alkyl group, amino group and nitro-group, and the coordinating element is one of molybdenum (Mo), tin (Sn), platinum (Pt), cobalt (Co), manganese (Mn) and titanium (Ti). The product disclosed by the invention uses the coating obtained from the organic coordination compound containing the elements, thus, can well resist acid, erosion of massive gas and impact of high current density, and has favorable cohesive property with the substrate; the service life of the electrode is prolonged; and the method is simple to operate, does not need complicated substrate pretreatment technology, and does not need a complicated middle layer or the like.
Description
Technical field
The present invention relates to a kind of electrode, specifically electrode coating and preparation method thereof.
Background technology
With metal titanium or other valve shaped metals is base material, with mixed metal oxide (being generally precious metal and other plain metal hopcalites) with electrocatalysis characteristic is the electrode of coating, and it is well-known being employed in a large number in industries such as multiple electrochemical field such as electrolysis, plating, chlor-alkali, organic electrosynthesis.This coated anode generally uses traditional thermal decomposition method, will contain the solution of catalytic performance metallics, and brushing in layer is on the process pure titanium plate of certain pre-treatment.By this method, combine non-metallurgical binding between the coating of acquisition and matrix.By the observation of scanning electron microscope, coating is irregular polygon cracking, and coating porosity is higher.Electrode in use can produce a large amount of gas, in some cases, in chlor-alkali or hypochlorite industry, is the target product of production or the target product of certain flow process; But in most industry, just exist, such as the oxygen or the chlorine of anode generation in the electroplating process as side reaction.The gassing reaction of this fierceness has produced bad influence for the life-span of coating, major cause is that these gases are when separating out from segmentation crack, the mechanical effect of fiercely washing away at the bubble of the formation of coatingsurface, especially in the higher environment of current density, the reaction of this intensive gassing may cause just existing originally that the coatings of a large amount of be full of cracks are easier phenomenon such as occurs peeling off, thereby has reduced the anodic life-span.Under the corrosive environment of routine, the corrosion resistance nature performance of catalyst coatings that contains precious metal is excellent unusually, even in the abominable electrolysis of most corrosive environment or electroplate under the environment and work, also has good superiority.And because the development of electrochemical industry is more and more harsher at some field environment, such as the thin copper foil field of electronic industry, or the zinc-plated industry of steel plate, because the needs of producing, anodic current density obviously strengthens.Under this environment, the oxygen evolution reaction is particularly violent, adds that working temperature is high again, and the phenomenon that the life-span obviously descends can appear in conventional noble metal electrode.
Summary of the invention
Problem at above-mentioned prior art existence, the purpose of this invention is to provide electrode coating of a kind of high-adhesiveness weather resistance and preparation method thereof, this electrode coating can improve the adhesivity of coating itself and base material, the segmentation crack number of coatingsurface is obviously reduced, compactness improves, thereby has prolonged the work-ing life of electrode.
To achieve these goals, technical scheme provided by the present invention is a kind of electrode coating of high-adhesiveness weather resistance, this electrode coating is added with coordination compound in iridium tantalum coating, wherein ligand is a kind of, two or three the combination in alkyl, amino and the nitro, and the coordination element is a kind of among molybdenum Mo, tin Sn, platinum Pt, cobalt Co, manganese Mn, the titanium Ti.
A kind of preparation method of electrode coating of high-adhesiveness weather resistance may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to g/ interpolation of metal iridium tantalum material loading total amount (0.8～1) thinner;
Step 2, be (5: 95)～(15: 85) according to coordination element in the coordination compound and iridium weight ratio, add coordination compound in the described solution of step 1, left standstill 1～2 hour after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used the degreaser oil removing after, at weight fraction is that 10～15% oxalic acid solution or volume fraction are digestion 1～3 hour in 50% the hydrochloric acid soln, use deionized water or distilled water to clean then, again with the raw spirit flushing, standby afterwards at air drying;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 100～150 ℃ of oven dry 10～15 minutes down, calcines 12～20 minutes down at 450～500 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 5, at last 450～500 ℃ of down calcinings 1～1.5 hour, obtain coating.
Beneficial effect: product of the present invention has used and has contained the coating that this element organic coordination compound obtains, and the impact of the washing away of acidproof, anti-a large amount of gases that can be fabulous, anti-high current density, with matrix good cohesiveness is arranged; Prolonged the work-ing life of electrode; Method is simple to operate, does not need complicated pretreatment of base material technology, does not need complicated middle layer etc.
Description of drawings
Fig. 1 is the sem photograph (* 2000 times) of various embodiments of the present invention 1;
Fig. 2 is the sem photograph (* 2000 times) of various embodiments of the present invention 2;
Fig. 3 is the sem photograph (* 2000 times) of various embodiments of the present invention 3;
Fig. 4 is the sem photograph (* 2000 times) of various embodiments of the present invention 4;
Fig. 5 is the sem photograph (* 2000 times) of various embodiments of the present invention 5;
Fig. 6 is the sem photograph (* 2000 times) of various embodiments of the present invention 6;
Fig. 7 is the sem photograph (* 2000 times) of comparative example.
Embodiment
Below in conjunction with the drawings and specific embodiments, further illustrate the present invention, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, should understand these embodiment and only be used to the present invention is described and be not used in and limit the scope of the invention.
Embodiment one: a kind of electrode coating of high-adhesiveness weather resistance, and this electrode coating is added with coordination compound in iridium tantalum coating, and wherein ligand is amino, and the coordination element is molybdenum Mo.
Its preparation method may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to 0.8g/ interpolation of metal iridium tantalum material loading total amount thinner propyl carbinol;
Step 2, according to coordination molybdenum in the coordination compound and iridium weight ratio 10: 90, in the described solution of step 1, add coordination compound, left standstill 1 hour after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used hot washing powder solution oil removing after, be digestion 3 hours in 10% the oxalic acid solution at weight fraction, use washed with de-ionized water then, again with the raw spirit flushing, standby afterwards at air drying;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 100 ℃ of oven dry 15 minutes down, calcines 12 minutes down at 500 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 5, at last 500 ℃ of down calcinings 1 hour, obtain coating.
Embodiment two: a kind of electrode coating of high-adhesiveness weather resistance, and this electrode coating is added with coordination compound in iridium tantalum coating, and wherein ligand is an alkyl, and the coordination element is tin Sn.
Its preparation method may further comprise the steps:
Step 1, at first be 30g/m2 configuration iridium tantalum masking liquid by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight, and according to 1g/ interpolation of metal iridium tantalum material loading total amount thinner propyl carbinol;
Step 2, to step 1 described solution in add coordination compound at 5: 95 according to coordination element tin in the coordination compound and iridium weight ratio, left standstill 1.5 hours after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used the oil removing of chemical reagent acetone after, be 50% hydrochloric acid soln digestion 1 hour in volume fraction, use distilled water to clean afterwards, and then with the raw spirit flushing, standby at air drying;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 110 ℃ of oven dry 13 minutes down, calcines 15 minutes down at 450 ℃ then, repetitive operation has repeatedly applied to masking liquid;
Step 5, at last 450 ℃ of down calcinings 1 hour, obtain coating.
Embodiment three: a kind of electrode coating of high-adhesiveness weather resistance, and this electrode coating is added with coordination compound in iridium tantalum coating, and wherein ligand is combination amino, nitro, and the coordination element is platinum Pt.
Its preparation method may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to 0.8g/ interpolation of metal iridium tantalum material loading total amount thinner propyl carbinol;
Step 2, be 8: 92 according to coordination elements platinum in the coordination compound and iridium weight ratio, add coordination compound in the described solution of step 1, left standstill 2 hours after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used the oil removing of chemical reagent acetone after, be digestion 1.5 hours in 13% the oxalic acid solution at weight fraction, use washed with de-ionized water then, again with the raw spirit flushing, treat that air drying is standby afterwards;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 120 ℃ of oven dry 15 minutes down, calcines 20 minutes down at 475 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 5, at last 480 ℃ of down calcinings 1 hour, obtain coating.
Embodiment four: a kind of electrode coating of high-adhesiveness weather resistance, and this electrode coating is added with coordination compound in iridium tantalum coating, and wherein ligand is combination amino, nitro, and the coordination element is cobalt Co.
Its preparation method may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to 0.8g/ interpolation of metal iridium tantalum material loading total amount thinner dehydrated alcohol;
Step 2, be 15: 85 according to coordination element cobalt in the coordination compound and iridium weight ratio, add coordination compound in the described solution of step 1, left standstill 1 hour after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used the oil removing of chemical reagent acetone after, be digestion 1 hour in 14% the oxalic acid solution at weight fraction, use washed with de-ionized water then, again with the raw spirit flushing, treat that air drying is standby afterwards;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 130 ℃ of oven dry 10 minutes down, calcines 15 minutes down at 480 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 5, at last 480 ℃ of down calcinings 1 hour, obtain coating.
Embodiment five: a kind of electrode coating of high-adhesiveness weather resistance, and this electrode coating is added with coordination compound in iridium tantalum coating, and wherein ligand is the combination of amino, alkyl and nitro, and the coordination element is manganese Mn.
Its preparation method may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to 0.9g/ interpolation of metal iridium tantalum material loading total amount thinner dehydrated alcohol;
Step 2, be 10: 90 according to coordination element manganese in the coordination compound and iridium weight ratio, add coordination compound in the described solution of step 1, left standstill 2 hours after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used hot washing powder solution oil removing after, be digestion 1 hour in 15% the oxalic acid solution at weight fraction, carry out deionized water rinsing then, again with the raw spirit flushing, treat that air drying is standby afterwards;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 140 ℃ of oven dry 10 minutes down, calcines 20 minutes down at 450 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 5, at last 480 ℃ of down calcinings 1.5 hours, obtain coating.
Embodiment six: a kind of electrode coating of high-adhesiveness weather resistance, and this electrode coating is added with coordination compound in iridium tantalum coating, and wherein ligand is a nitro, and the coordination element is titanium Ti.
Its preparation method may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to 1g/ interpolation of metal iridium tantalum material loading total amount thinner dehydrated alcohol;
Step 2, be 10: 90 according to coordination element titanium in the coordination compound and iridium weight ratio, add coordination compound in the described solution of step 1, left standstill 2 hours after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used the oil removing of chemical reagent acetone after, be digestion 1.5 hours in 50% the hydrochloric acid soln in volume fraction, carry out washed with de-ionized water then, afterwards again with raw spirit flushing, drying for standby;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 150 ℃ of oven dry 15 minutes down, calcines 20 minutes down at 450 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 5, at last 450 ℃ of down calcinings 1.5 hours, obtain coating.
Comparative example: a kind of conventional electrodes coating, this electrode coating are common iridium tantalum coating.
Its preparation method may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to 1g/ interpolation of metal iridium tantalum material loading total amount diluent ethanol, the masking liquid preparation finishes stand-by;
Step 2, the titanium base material used the degreaser oil removing after, be digestion 1 hour in 15% the oxalic acid solution at weight fraction, carry out deionized water rinsing then, afterwards again with raw spirit flushing, drying for standby;
Step 3, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 150 ℃ of oven dry 12 minutes down, calcines 10 minutes down at 500 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 4, at last 500 ℃ of down calcinings 1 hour, obtain coating.
The coated electrode of embodiment 1-6 and comparative example acquisition is cut into the sample that is of a size of 1cm*1cm, carry out the accelerated aging test as analysing oxygen anodes, in being the sulphuric acid soln of 1mol/L, concentration carries out the impact of the big electric current of 40kA/m2, to surpass starting voltage 8V as the test terminal point, test result sees Table 1.
Each embodiment of table 1 and comparative example electrode sample accelerated aging data
| Sequence | The accelerated aging value |
| Embodiment 1 | 2600h |
| Embodiment 2 | 1668h |
| Embodiment 3 | 1598h |
| Embodiment 4 | 2242h |
| Embodiment 5 | 1725h |
| Embodiment 6 | 1996h |
| Comparative example | 1574h |
Claims (4)
1. the electrode coating of a high-adhesiveness weather resistance, it is characterized in that: in iridium tantalum coating, be added with coordination compound, wherein ligand is a kind of, two or three the combination in alkyl, amino and the nitro, and the coordination element is a kind of among molybdenum Mo, tin Sn, platinum Pt, cobalt Co, manganese Mn, the titanium Ti.
2. the preparation method of the electrode coating of a high-adhesiveness weather resistance is characterized in that may further comprise the steps:
Step 1, at first be 30g/m by elemental indium tantalum Ir-Ta weight ratio 65: 35 and element gross weight
2Configuration iridium tantalum masking liquid, and according to g/ interpolation of metal iridium tantalum material loading total amount (0.8～1) thinner;
Step 2, be (5: 95)～(15: 85) according to coordination element in the coordination compound and iridium weight ratio, add coordination compound in the described solution of step 1, left standstill 1～2 hour after stirring fully, the masking liquid preparation finishes;
Step 3, the titanium base material used the degreaser oil removing after, at weight fraction is that 10～15% oxalic acid solution or volume fraction are digestion 1～3 hour in 50% the hydrochloric acid soln, use deionized water or distilled water to clean then, again with the raw spirit flushing, standby afterwards at air drying;
Step 4, with the titanium base material handled well with the masking liquid brushing that configures, brushing is finished the back 100～150 ℃ of oven dry 10～15 minutes down, calcines 12～20 minutes down at 450～500 ℃ then, repeatable operation has repeatedly applied masking liquid;
Step 5, at last 450～500 ℃ of down calcinings 1～1.5 hour, obtain coating.
3. according to the preparation method of the electrode coating of the described a kind of high-adhesiveness weather resistance of claim 2, it is characterized in that: thinner is dehydrated alcohol or propyl carbinol in the described step 1.
4. according to the preparation method of the electrode coating of the described a kind of high-adhesiveness weather resistance of claim 2, it is characterized in that: degreaser is hot washing powder solution or chemical reagent acetone in the described step 3.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104024481A (en) * | 2011-12-26 | 2014-09-03 | 培尔梅烈克电极股份有限公司 | High-load durable anode for oxygen generation and manufacturing method for the same |
| CN104289309A (en) * | 2014-10-16 | 2015-01-21 | 南通市崇川盛源净化器材厂 | Electric dust removal device and catalyst coating formula |
| CN105836854A (en) * | 2016-05-23 | 2016-08-10 | 张家富 | Water treatment device with wide application, water treatment electrode and manufacturing method for water treatment electrode |
| CN104480490B (en) * | 2014-12-08 | 2016-10-05 | 青岛双瑞海洋环境工程股份有限公司 | Ballast Management system cold water type oxide anode and preparation method |
| CN108002390A (en) * | 2017-11-30 | 2018-05-08 | 亚洲硅业（青海）有限公司 | A kind of electrode for reduction furnace and its coating production |
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| US7566389B2 (en) * | 2003-10-08 | 2009-07-28 | Akzo Nobel N.V. | Electrode |
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| CN1962471A (en) * | 2006-11-28 | 2007-05-16 | 北京科技大学 | Method for electrolyzing organic waste water using iridium tantalum stannum oxide coating titanium electrode |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104024481A (en) * | 2011-12-26 | 2014-09-03 | 培尔梅烈克电极股份有限公司 | High-load durable anode for oxygen generation and manufacturing method for the same |
| CN104289309A (en) * | 2014-10-16 | 2015-01-21 | 南通市崇川盛源净化器材厂 | Electric dust removal device and catalyst coating formula |
| CN104480490B (en) * | 2014-12-08 | 2016-10-05 | 青岛双瑞海洋环境工程股份有限公司 | Ballast Management system cold water type oxide anode and preparation method |
| CN105836854A (en) * | 2016-05-23 | 2016-08-10 | 张家富 | Water treatment device with wide application, water treatment electrode and manufacturing method for water treatment electrode |
| CN108002390A (en) * | 2017-11-30 | 2018-05-08 | 亚洲硅业（青海）有限公司 | A kind of electrode for reduction furnace and its coating production |
| CN108002390B (en) * | 2017-11-30 | 2019-02-05 | 亚洲硅业（青海）有限公司 | A kind of electrode for reduction furnace and its coating production |
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Address after: Zhongshan East Road, Baixia District of Nanjing city in Jiangsu province 210002 silk No. 472 building 4 floor Patentee after: Jiangsu Meite forestry special alloy Limited by Share Ltd Address before: Zhongshan East Road, Baixia District of Nanjing city in Jiangsu province 210002 silk No. 472 building 4 floor Patentee before: Metalink Special Alloys Corporation |