CN102330119A - Method for preparing high-purity porous iron film by adopting electrochemical method - Google Patents
Method for preparing high-purity porous iron film by adopting electrochemical method Download PDFInfo
- Publication number
- CN102330119A CN102330119A CN201110307707A CN201110307707A CN102330119A CN 102330119 A CN102330119 A CN 102330119A CN 201110307707 A CN201110307707 A CN 201110307707A CN 201110307707 A CN201110307707 A CN 201110307707A CN 102330119 A CN102330119 A CN 102330119A
- Authority
- CN
- China
- Prior art keywords
- acid
- preparation
- porous iron
- purity porous
- iron film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a preparation method of a high-purity porous iron film. According to the invention, an electrochemical method is adopted in the preparation method of the high-purity porous iron film. The preparation method is characterized in that size-reliable hydrogen bubbles formed on a substrate are taken as a template, and electroplating is carried out for a certain time period in an electroplating solution containing ferrous ions and hydrogen ions under the current density to form the high-purity porous iron film. In the invention, under the high current density which is higher than 0.5A/cm<2> and is less than 5A/cm<2>, the current density of 1-3A/cm<2> is preferably selected for electroplating, the ferrous ions can exist in inorganic salt and organic salt forms, the concentration of the ferrous ion is 0.1-0.5M preferably, the hydrogen ions can exist in inorganic acid and organic acid forms, the pH value of the electroplating solution is controlled to 0-2 preferably, electroplating time is 10-30 seconds preferably, and the concentration of a surfactant for controlling the sizes of the hydrogen bubbles is 0.05-0.5wt% preferably.
Description
Technical field
The present invention relates to the porous metal iron thin film, in particular to the method that obtains high-purity porous iron film through electrochemical means.
Background technology
Porous metal are to be metal inside disperse a large amount of directive or at random holes that distributing by a kind of low density functional materials that the metal particle of a large amount of dimensionings (or fiber) and microporosity constitute, and it has the 26S Proteasome Structure and Function double attribute.In laser inertial confinement nucleosynthesis (ICF) experiment, the radiation characteristic in target chamber is depended in the compression of pellet and implosion, so the target chamber seems most important in laser constraint nuclear fusion experimental.Because ferro element is the final product of nuclear fission and nucleosynthesis; The efficiency ratio of iron nuclear storage power is lighter all wants high with heavier element; Secondly owing to the high stability of iron in nuclear process, so it is the best materials in preparation inertial confinement fusion (ICF) igniting target chamber.
The preparation of porous metal film is divided into template and non-template method.With respect to the non-template method, template is the novel method that effectively prepares nano-porous materials, and the porous metal of preparation can be realized the relatively accurately control of its pattern and aperture size in this way.Template mainly comprises biological template method, colloidal crystal template, porous anodic alumina template method, pearl opal/counter opal structure template and bubble hydrogen template.Because the wall thickness of metal chamber target has only a few to tens of microns; The black chamber that method through mechanical workout in the non-template can't obtain to satisfy condition, and in template, the bubble hydrogen template is owing to uses bubble hydrogen not need preparation separately and removal as dynamic template; Other template then is difficult to remove (S.H.Glenzer; B.J.MacGowan, P.Michel, et al.Symmetric inertial confinement fusion implosions at ultra-high laser energies.Science.2010; 327:1228-1231), therefore can simply obtain three-dimensional porous metallic substance fast through the bubble hydrogen template.
Because irony is poor at the nature antioxidant property, the many forms with alloy of existing iron plating exist, at present domestic and international rarely seen bibliographical information and patented technology about preparing high-purity porous iron film.Therefore, we propose under high current density, utilize the structure of a large amount of bubble hydrogens of cathode hydrogen evolution reaction generation in the electrochemical deposition process as dynamic template completion porous iron.This template prepare the high purity iron thin-film process fast, technology simple controllable, with low cost, and can better satisfy the porous requirement of target chamber iron layer, be the feasibility method in preparation iron implosion target chamber.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing high-purity porous iron film.
Technical scheme of the present invention is: adopt the bubble hydrogen template to obtain high-purity porous iron film; It is characterized in that containing ferrous ion and hydrionic electroplate liquid; Under HCD, be template with the bubble hydrogen of the reliable size that in substrate, forms, make up high-purity porous iron film.
According to electroplate liquid of the present invention; Wherein, Ferrous ion can be inorganic salt and organic salt, and inorganic salt comprise iron protochloride, ferrous sulfate, ferrous ammonium sulphate etc., and organic salt comprises iron lactate, Iron diacetate etc.; The described salt concn scope that contains ferrous ion is 0.05M～1M, is preferably 0.1～0.5M.
According to electroplate liquid of the present invention, wherein, hydrogen ion can be mineral acid and organic acid; Mineral acid comprises hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid; Organic acid comprises carboxylic acid, sulfonic acid,-sulfinic acid etc., and the described pH value scope that contains hydrionic acid control plating bath is preferably 0～2 0～4.
According to electroplate liquid of the present invention; Wherein, The size of bubble hydrogen is realized by the tensio-active agent that adds plating bath; Tensio-active agent can be X 2073, sodium lauryl sulphate, OP-10, TX-10, trimethyl-glycine, and the described surfactant concentrations scope that contains is 0～1wt%, is preferably 0.05～0.5wt%.
The method of the high-purity porous iron film of electrochemical preparation of the present invention, it has used a large amount of bubble hydrogens as pore-forming material, it is characterized in that, and the current density in this plating bath is higher than 0.5A/cm
2And be 5A/cm
2Below, preferred 1～3A/cm
2, high current density causes the cathode height polarization to produce a large amount of pore-forming material bubble hydrogens.
In addition, in the electroplating process of high-purity porous iron of the present invention, the scope of electroplating time is 5s～60s, preferred 10s～30s.
According to the present invention,, utilize under the HCD through adopting above-mentioned formation; Cathode height polarization in the electrodeposition process; And, can constantly produce bubble hydrogen in the substrate with violent liberation of hydrogen process, reduction reaction can not take place on these bubble position occupied; The solution metal ion can only be in the hole between bubble " template " reduce deposition, thereby caused the generation in hole continuously in the settling.In addition, on hole wall, exist again and take measurements greatly less than the micropore of main aperture.
High-purity porous iron structure of the present invention's preparation has following characteristics and advantage:
1) porous iron of the present invention can obtain higher porosity, is interconnected between the hole, has a large amount of micropores on the hole wall again.
2) the present invention uses dynamic bubble hydrogen template to obtain the porous metallic substance, and template need not remove, preparing method's simple possible.In addition, the present invention does not have too much requirement, applied range to the selection of coating substrate.
3) the porous iron coating of the present invention's preparation is difficult for oxidation in physical environment, can obtain high-purity porous iron material.
Description of drawings
Fig. 1 is the scanning electron microscope diagram sheet of the high-purity porous iron different amplification of the present invention, has shown the microscopic appearance of high-purity porous iron, also shown simultaneously between the hole interconnect and hole wall on have a large amount of micropores.
Fig. 2 is the X ray diffracting spectrum of the high-purity porous iron of the present invention, has shown that the iron of preparation is high purity iron, and is not oxidized.
Embodiment
Below, carry out detailed explanation with regard to the preferred embodiment of the electro-plating method of high-purity porous iron film of the present invention.
Contain ferrous ion, hydrogen ion, tensio-active agent in the electroplate liquid of the present invention, and under HCD, carry out the short period of time and electroplate the high-purity porous iron film of acquisition.
As ferrous salt, so long as as the ferrous ion source of electroplate liquid and workman's ferrous salt all can use; Wherein, Ferrous ion can be inorganic salt and organic salt, and inorganic salt comprise iron protochloride, ferrous sulfate, ferrous ammonium sulphate etc., and organic salt comprises iron lactate, Iron diacetate etc.; The described salt concn scope that contains ferrous ion is 0.05M～1M, is preferably 0.1～0.5M.
As pH value of solution regulation and control person's hydrogen ion, so long as as the acid of regulating and control pH in the electroplate liquid, then all can use, wherein, hydrogen ion can be mineral acid and organic acid, and mineral acid comprises hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and organic acid comprises carboxylic acid, sulfonic acid.-sulfinic acid etc., the described pH value scope that contains hydrionic acid control plating bath is preferably 0～2 0～4.
In addition, add tensio-active agent in the plating bath of the present invention and can control the size of bubble hydrogen, thereby influence the pore size of high-purity porous iron coating.Tensio-active agent can be X 2073, sodium lauryl sulphate, OP-10, TX-10, trimethyl-glycine, and the described surfactant concentrations scope that contains is 0～1wt%, is preferably 0.05～0.5wt%.
In addition, the present invention is being higher than 0.5A/cm
2And be 5A/cm
2Under the following HCD, preferred 1～3A/cm
2Current density electroplate.Except high current density and common electrical are coated with the difference, the more common plating of electroplating time of the present invention is also had any different, and is controlled at 5s in the scope of 60s, preferred 10s～30s.
Before carrying out above-mentioned plating; To by the plating body, common pre-treatments such as mechanical polishing, degreasing, chemical rightenning can be implemented by ordinary method, among the present invention; As being had no particular limits by the plating body; So long as can implement the quilt plating body of iron plating usually, comprise gold and silver, copper, nickel, iron, cadmium, all can use.The operation of in addition, after plating, can implement to wash, alcohol being washed, nitrogen protection drying etc. is carried out usually.
Embodiment 1:
Electroplate liquid consists of: iron protochloride 0.1～0.3M, and hydrochloric acid control electroplate liquid pH 0～2, X 2073 0.05～0.5wt%, current density is selected 1～3A/cm
2Electroplating time 10～30s.The pore size of the high-purity porous iron film that obtains is about 5 μ m, and microscopic appearance is better.
Embodiment 2:
Electroplate liquid consists of: ferrous ammonium sulphate 0.1～0.3M, and sulfuric acid control electroplate liquid pH 0～2, sodium lauryl sulphate 0.05～0.5wt%, current density is selected 1～3A/cm
2Electroplating time 10～30s.The pore size of the high-purity porous iron film that obtains is about 3 μ m, and hole wall structure is better.
Embodiment 3:
Electroplate liquid consists of: Iron diacetate 0.1～0.3M, and carboxylic acid control electroplate liquid pH 0～2, OP-10 tensio-active agent 0.05～0.5wt%, current density is selected 1～3A/cm
2Electroplating time 10～30s.The pore size of the high-purity porous iron film that obtains is about 5 μ m, and the particle that constitutes hole wall structure is less.
Claims (9)
1. the preparation method of a high-purity porous iron film; It is characterized in that containing ferrous ion and hydrionic electroplate liquid; Under HCD, be template with the bubble hydrogen of the reliable size that in substrate, forms, form high-purity porous iron film through electroplating in the regular hour scope.
2. the preparation method of high-purity porous iron film according to claim 1, wherein, ferrous ion can be inorganic salt and organic salt, and inorganic salt comprise iron protochloride, ferrous sulfate, ferrous ammonium sulphate etc., and organic salt comprises iron lactate, Iron diacetate etc.
3. the preparation method of high-purity porous iron film according to claim 1, wherein, hydrogen ion can be mineral acid and organic acid, and mineral acid comprises hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and organic acid comprises carboxylic acid, sulfonic acid,-sulfinic acid.
4. the preparation method of high-purity porous iron film according to claim 1, wherein, current density range is 0.5A/cm
2～5A/cm
2Below, preferred 1～3A/cm
2Current density electroplate, the electroplating time scope is 5s～60s, preferred 10s～30s.
5. the preparation method of high-purity porous iron film according to claim 1; Wherein, The size of bubble hydrogen realizes that by the tensio-active agent that adds plating bath tensio-active agent can be X 2073, sodium lauryl sulphate, OP-10, TX-10, trimethyl-glycine.
6. the preparation method of high-purity porous iron film according to claim 1, wherein, base metal comprises gold and silver, copper, nickel, iron, cadmium.
7. the salt concn scope that contains ferrous ion according to claim 2 is 0.05M～1M, is preferably 0.1～0.5M.
8. the pH value scope that contains hydrionic acid control plating bath according to claim 3 is preferably 0～2 0～4.
9. the surfactant concentrations scope that contains according to claim 2 is 0～1wt%, is preferably 0.05～0.5wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110307707A CN102330119A (en) | 2011-10-12 | 2011-10-12 | Method for preparing high-purity porous iron film by adopting electrochemical method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110307707A CN102330119A (en) | 2011-10-12 | 2011-10-12 | Method for preparing high-purity porous iron film by adopting electrochemical method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102330119A true CN102330119A (en) | 2012-01-25 |
Family
ID=45482077
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110307707A Pending CN102330119A (en) | 2011-10-12 | 2011-10-12 | Method for preparing high-purity porous iron film by adopting electrochemical method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102330119A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634823A (en) * | 2012-05-17 | 2012-08-15 | 云南民族大学 | Preparation method of micro porous iron foil |
| CN103046088A (en) * | 2012-12-20 | 2013-04-17 | 华南理工大学 | Micro-nano composite porous copper surface structure and preparation method and device thereof |
| CN103132111A (en) * | 2013-01-25 | 2013-06-05 | 重庆大学 | Preparation method of three-dimensional micrometer level porous copper thin film |
| CN103274354A (en) * | 2013-05-17 | 2013-09-04 | 哈尔滨工业大学 | Preparation method of gecko structure simulating adhesive |
| CN103849910A (en) * | 2014-03-26 | 2014-06-11 | 哈尔滨工业大学 | Preparation method of super-hydrophobic meshy material |
| CN104934238A (en) * | 2015-06-25 | 2015-09-23 | 东南大学 | Method for preparing porous graphene electrode material by air bubble template process and application of method |
| CN105839153A (en) * | 2016-05-25 | 2016-08-10 | 上海交通大学 | Preparing method for high-electricity-conductivity and high-infrared-emissivity film layer on surface of magnesium alloy |
| CN106207596A (en) * | 2016-06-28 | 2016-12-07 | 杭州华锦电子有限公司 | A kind of seal wiring seat injection process |
| CN106757174A (en) * | 2017-02-23 | 2017-05-31 | 黄芃 | A kind of electro-deposition prepares the method and device of metal dust |
| CN108118360A (en) * | 2017-12-26 | 2018-06-05 | 东华大学 | A kind of efficiently production formic acid Cu-Sn-Cu layered laminate foam electrodes and preparation method thereof |
| CN110424021A (en) * | 2019-07-19 | 2019-11-08 | 陕西理工大学 | A kind of method that electrochemistry prepares di-iron trioxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2716325B2 (en) * | 1992-08-24 | 1998-02-18 | 株式会社 イケックス工業 | Metal electrodeposition method |
| WO2006068444A1 (en) * | 2004-12-23 | 2006-06-29 | Seoul National University Industry Foundation | Fabrication of mesoporous metal electrodes in non-liquid-crystalline phase and its application |
| WO2011090279A2 (en) * | 2010-01-22 | 2011-07-28 | Bioneer Corporation | Porous films comprising carbon nanostructure-metal composite and method of manufacturing the same |
-
2011
- 2011-10-12 CN CN201110307707A patent/CN102330119A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2716325B2 (en) * | 1992-08-24 | 1998-02-18 | 株式会社 イケックス工業 | Metal electrodeposition method |
| WO2006068444A1 (en) * | 2004-12-23 | 2006-06-29 | Seoul National University Industry Foundation | Fabrication of mesoporous metal electrodes in non-liquid-crystalline phase and its application |
| WO2011090279A2 (en) * | 2010-01-22 | 2011-07-28 | Bioneer Corporation | Porous films comprising carbon nanostructure-metal composite and method of manufacturing the same |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634823A (en) * | 2012-05-17 | 2012-08-15 | 云南民族大学 | Preparation method of micro porous iron foil |
| CN102634823B (en) * | 2012-05-17 | 2014-08-13 | 云南民族大学 | Preparation method of micro porous iron foil |
| CN103046088B (en) * | 2012-12-20 | 2015-08-26 | 华南理工大学 | A kind of micro-nano compound porous copper surface tissue and preparation method thereof and device |
| CN103046088A (en) * | 2012-12-20 | 2013-04-17 | 华南理工大学 | Micro-nano composite porous copper surface structure and preparation method and device thereof |
| CN103132111A (en) * | 2013-01-25 | 2013-06-05 | 重庆大学 | Preparation method of three-dimensional micrometer level porous copper thin film |
| CN103132111B (en) * | 2013-01-25 | 2015-05-27 | 重庆大学 | Preparation method of three-dimensional micrometer level porous copper thin film |
| CN103274354A (en) * | 2013-05-17 | 2013-09-04 | 哈尔滨工业大学 | Preparation method of gecko structure simulating adhesive |
| CN103274354B (en) * | 2013-05-17 | 2015-07-01 | 哈尔滨工业大学 | Preparation method of gecko structure simulating adhesive |
| CN103849910A (en) * | 2014-03-26 | 2014-06-11 | 哈尔滨工业大学 | Preparation method of super-hydrophobic meshy material |
| CN103849910B (en) * | 2014-03-26 | 2016-04-13 | 哈尔滨工业大学 | A kind of preparation method of netted super hydrophobic material |
| CN104934238A (en) * | 2015-06-25 | 2015-09-23 | 东南大学 | Method for preparing porous graphene electrode material by air bubble template process and application of method |
| CN105839153A (en) * | 2016-05-25 | 2016-08-10 | 上海交通大学 | Preparing method for high-electricity-conductivity and high-infrared-emissivity film layer on surface of magnesium alloy |
| CN105839153B (en) * | 2016-05-25 | 2018-10-23 | 上海交通大学 | The preparation method of Mg alloy surface high conductivity high IR emissivity film layer |
| CN106207596A (en) * | 2016-06-28 | 2016-12-07 | 杭州华锦电子有限公司 | A kind of seal wiring seat injection process |
| CN106757174A (en) * | 2017-02-23 | 2017-05-31 | 黄芃 | A kind of electro-deposition prepares the method and device of metal dust |
| CN108118360A (en) * | 2017-12-26 | 2018-06-05 | 东华大学 | A kind of efficiently production formic acid Cu-Sn-Cu layered laminate foam electrodes and preparation method thereof |
| CN110424021A (en) * | 2019-07-19 | 2019-11-08 | 陕西理工大学 | A kind of method that electrochemistry prepares di-iron trioxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102330119A (en) | Method for preparing high-purity porous iron film by adopting electrochemical method | |
| Cherevko et al. | Impact of key deposition parameters on the morphology of silver foams prepared by dynamic hydrogen template deposition | |
| Cherevko et al. | Hydrogen template assisted electrodeposition of sub-micrometer wires composing honeycomb-like porous Pb films | |
| Lotfi et al. | Surface modification of Ni foam by the dendrite Ni-Cu electrode for hydrogen evolution reaction in an alkaline solution | |
| CN103173840A (en) | Method for producing grinding electroplated diamond wheel | |
| US20190010627A1 (en) | Method for treating a surface of a metallic structure | |
| CN103132111B (en) | Preparation method of three-dimensional micrometer level porous copper thin film | |
| Haehnel et al. | Electrodeposition of Fe70Pd30 nanowires from a complexed ammonium–sulfosalicylic electrolyte with high stability | |
| CN100449038C (en) | Process for preparing invor alloy foil | |
| KR102176791B1 (en) | Method for manufacturing aluminum anodic oxide film having pillar-on-pore structure using phosphoric acid | |
| Wu et al. | Enhanced electrochemical performance of nickel hydroxide electrode with monolayer hollow spheres composed of nanoflakes | |
| CN103481583B (en) | A kind of surface has the preparation method processing Copper Foil of loose structure | |
| CN103397349A (en) | Preparation method of two-dimensional feathery copper powder under ammonia condition | |
| Nagaura et al. | Fabrication of ordered Ni nanocones using a porous anodic alumina template | |
| Koboski et al. | Hydrogen evolution reaction measurements of dealloyed porous NiCu | |
| CN104593786A (en) | Method for microporous treatment of metal surface | |
| Miao et al. | Recent progress and prospect of electrodeposition-type catalysts in carbon dioxide reduction utilizations | |
| CN102747406A (en) | Magnesium alloy anodic oxidation electrolyte and magnesium alloy surface treatment method | |
| CN110144620A (en) | A kind of selection laser melting molding stainless steel surface nano pipe array preparation method | |
| CN104894614B (en) | A kind of electroplate liquid and electro-plating method producing nickel plating thorn abrasive grain | |
| Trofimova et al. | The dynamics of the nickel foam formation and its effect on the catalytic properties toward hydrogen evolution reaction | |
| Sivasubramanian et al. | Boric acid assisted electrosynthesis of hierarchical three-dimensional cobalt dendrites and microspheres | |
| Abbar et al. | Electrochemical preparation of ultrafine zinc powder | |
| Yue et al. | Hierarchical structured nickel–copper hybrids via simple electrodeposition | |
| CN103243356A (en) | Preparation method of iron-nickel-cobalt-molybdenum alloy foil by electrodeposition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120125 |