CN100422392C - Electrochemical polish process for nickel-base strip for preparing coating superconductor - Google Patents
Electrochemical polish process for nickel-base strip for preparing coating superconductor Download PDFInfo
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- CN100422392C CN100422392C CNB2004100836185A CN200410083618A CN100422392C CN 100422392 C CN100422392 C CN 100422392C CN B2004100836185 A CNB2004100836185 A CN B2004100836185A CN 200410083618 A CN200410083618 A CN 200410083618A CN 100422392 C CN100422392 C CN 100422392C
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Abstract
The present invention relates to an electrochemical polish process method for a nickel-base strip for preparing a coating superconductor, which can decrease the roughness of the surface of the nickel-base strip for preparing a coating superconductor. The process comprises that (1) phosphoric acid and glycerin of which the volume ratio is (95 to 105): (0.1 to 0.5) prepare electrochemical polish liquid, wherein the concentration of the phosphoric acid is 85%; (2) the electrochemical polish liquid which is prepared by the step (1) as electrolysis liquid, a nickel-base strip for preparing a coating superconductor as anode material, and stainless steel as cathode material are submerged in the electrochemical polish liquid; a power supply is switched on; the polish can be carried out under the conditions of the voltage of 5 V to 10 V and the current of 0.3A to 1A; the polish time is controlled within the range of 10 minutes to 60 minutes; (3) after polish, the nickel-base strip for preparing a coating superconductor is cleaned and blown for drying. The roughness of the surface of the nickel-base strip after processed by the technology is about more than ten nanometers, which can satisfy preparing requirements of a coating superconductor.
Description
Technical field
The invention belongs to coating superconductor preparation and surface finish processing technology field.The present invention relates to a kind of electrochemical etching processing method of coating superconductor nickel-base strip.
Background technology
Coating superconductor mainly refers to the YBCO coating conductor, and the preparation characteristic of such material mainly is: (1) is base material with the flexible metal band, mainly is with the nickel sheet metal strip with high cubic texture degree rolling and that the recrystallize heat treating method obtains; (2) one or more layers oxide-isolation layer of deposition on metal base band, this sealing coat stops the nickel metal to spread in YBCO on the one hand, require to have cubic texture on the other hand, can induce the YBCO on it to form texture, the selection of insolated layer materials requires lattice parameter, thermal expansivity and metal base close with YBCO, and Heat stability is good; (3) on sealing coat, deposit YBCO superconducting layer with cubic texture.
Public publication about " YBCO coating conductor " has: " epitaxy YBCO on biaxial texture (001) nickel: a kind of approach that obtains the high current density superconducting tape " [Science (science magazine), 274 (1996) 755] (D.P.Norton, A.Goyal, J.D.Budai, D.K.Christen, D.M.kroeger, E.D.Specht, Q.He, B.Saffian, M.Paranthaman, C.E.Klabunde, D.F.Lee and F.A.list); " metal and the oxide-isolation layer of deposition diaxial orientation on the texture nickel-base strip: a kind of matrix that is used for the high current density high-temperature superconductor " [Physica C, 275 (1997), 155] (Qing He, Christen D K, Budai J D, Lee D F, Goyal A, Norton DP, Paranthaman M, List F A and Kyoeger D M).
Public publication about " coating superconductor nickel-base strip " has: " non-magnetic cubic woven structure copper-nickel alloy base band ", Chinese patent application number: 01141893.1; " preparation method of cubic texture Ni base band ", Chinese patent application numbers 97121916.8.
In above three steps, the first step is most important, and it has determined the coating superconductor final properties to a great extent.The nickel metal base band mainly influences the performance of whole coating superconductor aspect two of cubic texture intensity and surfacenesses.Aspect cubic texture intensity,, can obtain the very high base band of cubic texture intensity by continuing to optimize rolling and the recrystallize thermal treatment process.And reducing aspect the base band surfaceness, beautiful, a day company utilizes its advanced minute surface roller rolling machine can be with the base band Roughness Surface on Control under tens nanometers, thereby greatly improves the coating superconductor performance.China is subjected to the restriction of milling equipment level, is difficult to the base band of preparation surfaceness less than tens nanometers, and this becomes the one of the main reasons that hinders China's coating superconductor level raising.The present invention's expectation utilizes glossing that the surfaceness of nickel-base strip is decreased to tens nanometers, satisfies the requirement of preparation coating superconductor.
Industrially generally reduce workpiece surface roughness with glossing, using more glossing has mechanical polishing, chemical rightenning and electrochemical etching.Mechanical polishing be by the polishing wheel that is wiped with rubbing paste of high speed rotating to improve the mechanical processing process of metallic article surfacing and bright degree, it can cause that viscous deformation takes place on the metal works surface, and can produce tissue variation because of local heating.Chemical rightenning is that metal works is handled process smooth to obtain, glossy surface in certain solution, generally follows more violent chemical reaction, and process is wayward, and the polishing fluid life-span is shorter.Electrochemistry (electrolysis) polishing be with workpiece as anode 12, insoluble petal (or inert conductor) immerses simultaneously as negative electrode 13, two electrodes and passes to direct current in the electrolyzer and produce anodic dissolution processes selectively, sees accompanying drawing 1.In the electrochemical etching process, the electrolyte layer 14 of close anode 12 forms the full-bodied metal-salt film of one deck (being mucous membrane) on workpiece surface.On the rough anode metal surface, the viscosity of its mucous layer, thickness, proportion etc. are all inequality, the mucous layer of bossing is thin than recess, resistance ratio is less, current density is bigger, so accelerated the dissolving of bossing metal, bossing is gradually smooth, reach the smooth smooth purpose on surface at last.
The domestic coating superconductor preparation suitability for industrialized production that still is unrealized still is in the exploratory stage so comprise a large amount of technical tasks such as nickel-base strip polishing, not have the patent of discovery about coating superconductor nickel-base strip glossing at present.
Summary of the invention
The electrochemical etching processing method that the purpose of this invention is to provide a kind of coating superconductor nickel-base strip, utilize this electrochemical etching processing method can reduce coating superconductor metallic nickel base band surfaceness to tens nanometer, thereby enable to satisfy the requirement of coating superconductor preparation.
For achieving the above object, the present invention takes following technical scheme:
A kind of electrochemical etching processing method of coating superconductor nickel-base strip is characterized in that: this method comprises the steps:
(1), be 95-105: 0.1-0.5 with the volume ratio of phosphoric acid and glycerol, the preparation electrochemical polish liquid, wherein, concentration of phosphoric acid is 85%;
(2), with the electrochemical polish liquid of step (1) preparation as electrolytic solution, with the coating superconductor nickel-base strip as anode material, stainless steel is as cathode material, be immersed in the electrochemical polish liquid, connect power supply, at 5～10V voltage, to polish in 0.3～1A electric current, the time was controlled at 10～60 minutes;
(3), after the polishing, the coating superconductor nickel substrate is cleaned, dries up.
In the electrochemical etching processing method of coating superconductor nickel-base strip of the present invention, the coating superconductor nickel-base strip that uses in the described step (2) is through the coating superconductor nickel-base strip with high cubic texture degree rolling and that the recrystallize heat treating method obtains.
In the electrochemical etching processing method of coating superconductor nickel-base strip of the present invention, the coating superconductor nickel-base strip with high cubic texture degree that uses in the described step (2) will carry out pre-treatment earlier before polishing, this pre-treatment comprises that the time respectively is 8-15 minute with the ultrasonic oil removing of acetone with two processes of deionized water ultrasonic cleaning.Like this, guarantee the surface quality of the preceding nickel-base strip of polishing, make base band keep surfacing, cleaning oil stains-less.
In the electrochemical etching processing method of coating superconductor nickel-base strip of the present invention, in the described step (2), the area of stainless cathode material is more than or equal to the area of the anode material of coating superconductor nickel-base strip.
In the electrochemical etching processing method of coating superconductor nickel-base strip of the present invention, in the described step (3), the coating superconductor nickel substrate after the polishing is to clean in distilled water.
In the electrochemical etching processing method of coating superconductor nickel-base strip of the present invention, in the described step (3), in polishing process, note keeping the temperature-stable of electrochemical polish liquid in room temperature.
In the electrochemical etching processing method of coating superconductor nickel-base strip of the present invention, be to be main raw material with phosphoric acid, be auxiliary material with the glycerol additive, be mixed with transparent, stable electrochemical polish liquid.
In the electrochemical etching processing method of coating superconductor nickel-base strip of the present invention, in described step (2), polishing time is controlled according to polishing workpiece size, voltage and current size, and polishing time generally was controlled at 10～60 minutes.
The invention provides a kind of electrochemical etching processing method that reduces coating superconductor texture nickel-base strip surfaceness.Can make the surfaceness of texture metal base band be decreased to tens nanometers with the inventive method, can satisfy the requirement of coating superconductor preparation.This invention well below the investment of purchasing the high quality mirror roller rolling machine, is expected to promote coating superconductor research and industrialized development thereof on cost.
Description of drawings
Fig. 1 is common electrochemical polish apparatus synoptic diagram
Fig. 2 is Ni base band (111) utmost point figure
Fig. 3 is Ni base band electrochemical etching rear surface AFM figure
Fig. 4 is electrochemical polish apparatus figure of the present invention
Embodiment
Be one embodiment of the present of invention below, the present invention is not limited to this embodiment.
Get texture nickel metal base band, (20 * 30cm) carry out pre-treatment to be cut into sample.Detailed process is that elder generation's ultrasonic cleaning in acetone was put into deionized water for ultrasonic and cleaned 10 minutes to reach the purpose of oil removing in 10 minutes then, and it is standby to put into raw spirit after finishing.This Ni substrate has very strong cubic texture (as shown in Figure 2) owing to passed through special rolling and recrystallize thermal treatment process.
Measure 100ml phosphoric acid (concentration 85%), add the 0.5ml glycerol, fully stir, be mixed with electrochemical polish liquid, place in the beaker.
Electrochemical polish apparatus is got a power supply 1 as shown in Figure 4, the nickel-base strip sample is linked to each other with power anode by lead, as anode 2.(30 * 30cm) are connected with power supply by lead, as negative electrode 3 with stainless steel substrate.The anode and cathode material all is immersed in the electrochemical polish liquid 4 for preparing, forms complete electrochemical polish apparatus, prepare polishing.
Power-on is stabilized in 7V with voltage, and electric current 0.5A, electrochemical etching begin to carry out, and polishing time was controlled at 20 minutes.
After polishing finishes, powered-down.The base band sample is taken off cleaning in distilled water, dried up, and so far electrochemical etching finishes.
Base band atomic force microscope observation behind the electrochemical etching, as shown in Figure 3, Fig. 3 is the atomic force microscope picture (AFM) on base band surface behind the electrochemical etching, and is comparatively smooth by the picture visible surface, surfaceness is about tens nanometers, can satisfy the requirement of coating superconductor.
Claims (5)
1. the electrochemical etching processing method of a coating superconductor nickel-base strip, it is characterized in that: this method comprises the steps:
(1), be 95-105: 0.1-0.5 with the volume ratio of phosphoric acid and glycerol, the preparation electrochemical polish liquid, wherein, concentration of phosphoric acid is 85%;
(2), with the electrochemical polish liquid of step (1) preparation as electrolytic solution, with the coating superconductor nickel-base strip as anode material, stainless steel is as cathode material, be immersed in the electrochemical polish liquid, connect power supply, at 5～10V voltage, to polish in 0.3～1A electric current, the time was controlled at 10～60 minutes;
(3), after the polishing, the coating superconductor nickel substrate is cleaned, dries up.
2. the electrochemical etching processing method of coating superconductor nickel-base strip according to claim 1, it is characterized in that: the coating superconductor nickel-base strip that uses in the described step (2) is through the coating superconductor nickel-base strip with high cubic texture degree rolling and that the recrystallize heat treating method obtains.
3. as the electrochemical etching processing method of coating superconductor nickel-base strip as described in the claim 2, it is characterized in that: the coating superconductor nickel-base strip with high cubic texture degree that uses in the described step (2) will carry out pre-treatment earlier before polishing, this pre-treatment comprises that the time respectively is 8-15 minute with the ultrasonic oil removing of acetone with two processes of deionized water ultrasonic cleaning.
4. as the electrochemical etching processing method of coating superconductor nickel-base strip as described in claim 2 or 3, it is characterized in that: in the described step (2), the area of stainless cathode material is more than or equal to the area of the anode material of coating superconductor nickel-base strip.
5. as the electrochemical etching processing method of coating superconductor nickel-base strip as described in the claim 4, it is characterized in that: in the described step (3), the coating superconductor nickel substrate after the polishing is to clean in distilled water.
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| CNB2004100836185A CN100422392C (en) | 2004-10-13 | 2004-10-13 | Electrochemical polish process for nickel-base strip for preparing coating superconductor |
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| CNB2004100836185A CN100422392C (en) | 2004-10-13 | 2004-10-13 | Electrochemical polish process for nickel-base strip for preparing coating superconductor |
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| CN100422392C true CN100422392C (en) | 2008-10-01 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013002410A1 (en) * | 2011-06-30 | 2013-01-03 | 古河電気工業株式会社 | Superconducting thin film substrate and superconducting thin film, and superconducting thin film substrate manufacturing method |
| CN102494933B (en) * | 2011-11-28 | 2013-09-18 | 山东大学 | Corrosive for showing white layer of processed surface of nickel-base superalloy as well as preparation method and applications thereof |
| CN103938148B (en) * | 2014-04-09 | 2016-11-23 | 西南交通大学 | A kind of method preparing conductor of high-temperature superconductor coat NiO cushion in atmosphere |
| CN104532338A (en) * | 2014-12-11 | 2015-04-22 | 沈阳富创精密设备有限公司 | Hastelloy electrolytic polishing process |
| CN105568358B (en) * | 2016-03-21 | 2017-08-29 | 苏州新材料研究所有限公司 | For the electrochemical polish liquid of Hastelloy base band, preparation method and polishing method |
| CN107119313A (en) * | 2017-03-01 | 2017-09-01 | 西北大学 | A kind of electrochemical polishing method and method for preparing graphene membrane |
| CN110578164A (en) * | 2018-06-11 | 2019-12-17 | 深圳市裕展精密科技有限公司 | Electrochemical polishing electrolyte for titanium and titanium alloy and use method thereof |
| CN110205670B (en) * | 2019-07-10 | 2020-09-08 | 二重（德阳）重型装备有限公司 | Corrosion inhibition nickel-based alloy electrolytic polishing solution and polishing method thereof |
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| RU1832138C (en) * | 1990-12-27 | 1993-08-07 | Московский вечерний металлургический институт | Electrolyte for metal polishing |
| CN1107904A (en) * | 1994-12-29 | 1995-09-06 | 华中理工大学 | Electrochemical polishing method for aluminum or aluminum alloy welding wire |
| JPH08302500A (en) * | 1995-05-02 | 1996-11-19 | Electroplating Eng Of Japan Co | Electropolishing solution for platinum and platinum alloy |
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Patent Citations (5)
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| JPS54103746A (en) * | 1978-02-02 | 1979-08-15 | Matsushita Electric Ind Co Ltd | Method of electropolishing sendust |
| RU1832138C (en) * | 1990-12-27 | 1993-08-07 | Московский вечерний металлургический институт | Electrolyte for metal polishing |
| CN1107904A (en) * | 1994-12-29 | 1995-09-06 | 华中理工大学 | Electrochemical polishing method for aluminum or aluminum alloy welding wire |
| JPH08302500A (en) * | 1995-05-02 | 1996-11-19 | Electroplating Eng Of Japan Co | Electropolishing solution for platinum and platinum alloy |
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| ACTIVE, PASSIVE AND TRANSPASSIVE DISSOLUTIONOF A NICKEL-BASE SUPER ALLOY IN CONCENTRATEDACID MIXTURE SOLUTION. SINGH VB, ARVIND U.WERKSTOFFE UND KORROSION-MATERIALS AND CORROSION,Vol.46 No.10. 1995 * |
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Effective date of registration: 20190626 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |
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