EP1913181B1 - Procede d'electropolissage - Google Patents

Procede d'electropolissage Download PDF

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Publication number
EP1913181B1
EP1913181B1 EP06776534.7A EP06776534A EP1913181B1 EP 1913181 B1 EP1913181 B1 EP 1913181B1 EP 06776534 A EP06776534 A EP 06776534A EP 1913181 B1 EP1913181 B1 EP 1913181B1
Authority
EP
European Patent Office
Prior art keywords
electrolyte
phosphoric acid
rinsing
acid
electropolishing
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.)
Not-in-force
Application number
EP06776534.7A
Other languages
German (de)
English (en)
Other versions
EP1913181A1 (fr
Inventor
Siegfried Piesslinger-Schweiger
Olaf BÖHME
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Poligrat GmbH
Original Assignee
Poligrat GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Poligrat GmbH filed Critical Poligrat GmbH
Publication of EP1913181A1 publication Critical patent/EP1913181A1/fr
Application granted granted Critical
Publication of EP1913181B1 publication Critical patent/EP1913181B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/16—Polishing
    • C25F3/22—Polishing of heavy metals
    • C25F3/24—Polishing of heavy metals of iron or steel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
    • C25F7/02—Regeneration of process liquids

Definitions

  • the present invention describes a method for the electrochemical polishing of workpieces made of steel, in which an etching of the surface during the flushing process can be avoided without the use of costly and environmentally harmful inhibitors.
  • This method is particularly suitable for workpieces made of low-alloyed steels, which are particularly vulnerable to chemical attack.
  • Electrochemical polishing is a process that is used to deburr, smooth and shine metal surfaces. Due to the higher current density of fine scratches and other unevenness, the metal ionizes and dissolves faster at these points than at the smooth areas of a metal workpiece, thereby compensating its unevenness.
  • the objects to be electropolished which are suspended from corresponding support elements or arranged in baskets or the like, are immersed in an electrolyte, the polishing bath, and lifted out of the latter after a certain time. After draining the bath liquid from the polished surfaces, the articles are immersed in rinsing baths to completely remove the electrolyte.
  • chromic acid ie an oxo acid of hexavalent chromium (chromate)
  • chromate hexavalent chromium
  • Chromates are highly toxic, teratogenic and carcinogenic, which is why their use in the industry is increasingly limited and subject to high safety standards in terms of occupational safety and environmental protection.
  • the patent JP-A 5 163 600 describes the addition of ascorbic acid or salts of ascorbic acid as a way to reduce the hexavalent chromate to chromium (III) ions, which are less toxic.
  • chromic acid also represents a significant cost factor that further restricts the economics of the electropolishing process.
  • Decisive for the gloss and smoothness of the machined article is the flushing process following the electropolishing step, which is intended to clean the surfaces of the adhering electrolyte.
  • the resulting reduction in the concentration of the acid on the surface of the electropolished article increases the corrosive effect of the electrolyte. This effect is to be suppressed by the addition of inhibitors such as chromic acid. Without these additions, the freshly polished metal surfaces are again etched, whereby the effect achieved by the electropolishing of smoother and glossier surfaces is lost to a considerable extent.
  • the DE 808 519 B describes a process for polishing and deburring high or low carbon and low alloy steels electrolytically.
  • the Electrolyte contains 5 to 60 wt .-% sulfuric acid and 30 to 80 wt .-% phosphoric acid.
  • the electrolyte bath may additionally contain a trivalent dissolved metal, such as iron.
  • the AT 190 769 B describes a method and an electrolyte for the electrolytic cleaning of metal objects.
  • the electrolyte consists of hydrochloric acid and after the electrolysis is rinsed, the phosphoric acid in the ratio of about 0.05% to 3% can be added to the rinse water.
  • This phosphoric acid additive serves the purpose of preventing the formation of oxides on the metal of the treated article.
  • the DE 808 519 C describes a process for polishing and deburring high or low carbon and low alloy steels electrolytically.
  • the GB 835 594 A relates to a method of treating wires.
  • the GB 601 980 A describes an electrolytic process using sulfuric acid and phosphoric acid.
  • the invention presented here is based on an electropolishing method which, like the electropolishing method for stainless steel, is based on mixtures of phosphoric acid and sulfuric acid, the first rinsing step with phosphoric acid-containing solution following the actual electropolishing step with a solution having a phosphoric acid content of at least 50% by weight , is carried out.
  • the use of concentrated phosphoric acid, which contains a proportion of 85 wt.% H 3 PO 4 is suitable here as a starting solution. This process does not require the addition of chromic acid or other inhibitors and therefore offers significant, not only economic benefits.
  • the articles to be electro-polished are degreased in an optional step to avoid contamination of the electrolyte and to make the surfaces of the workpieces completely accessible to the electrolyte.
  • any commercial degreasing solution can be used.
  • the workpieces are usually rinsed with water and then immersed in the electropolishing and anodized.
  • An undesirable chemical attack on the surfaces of the electropolishing article may be inhibited during the electropolishing step by keeping the water content of the electrolytes low. Therefore, almost exclusively highly concentrated acids such as sulfuric acid, phosphoric acid and mixtures of sulfuric acid and phosphoric acid are used for the electropolishing of steels and steel alloys. Particularly good effect show thereby electrolytes, which have a water content of at most 20 wt.%.
  • the temperature of the electrolyte should be above 50 ° C, preferably 60 ° C to 90 ° C.
  • the iron ions removed from the workpiece surface during the electropolishing process dissolve in the electrolyte and are enriched there. Beyond a critical concentration of about 8% by weight, corresponding to about 140 grams per liter of iron in the electrolyte, the effectiveness of the electrolyte decreases markedly. This requires a reduction of the iron content by partial exchange with fresh electrolyte.
  • the removal of the spent electrolyte can be done both directly, as well as by extraction in the rinsing process.
  • the withdrawn used electrolyte must either be returned to an authorized location for destruction or made ready for use by regeneration.
  • the electrolytic precipitation of the iron in the form of Fe (II) sulfate from the concentrated electrolyte is outstandingly suitable.
  • waste from the electropolishing process ultimately only the removed iron in the form of iron (II) sulfate falls which, in turn, can be further used industrially as a reducing agent.
  • a set of tools hardened tool steel (material no. 1.3343) was in an electrolyte consisting of 50 parts by weight of phosphoric acid and 50 parts by weight of sulfuric acid having a specific gravity of 1.75 kg / l and an iron content of 4.5 wt .% at an electrolyte temperature of 80 ° C, a current density of 40 A / dm 2 and a voltage of 12 V for a period of 6 min electropolished and then pre-rinsed in concentrated phosphoric acid (85 wt.%) at room temperature, rinsed in water, then dipped in water at a temperature of 60 ° C, to which a commercial corrosion inhibitor in a concentration of 2 wt.% Was added, and dried in air.
  • a second set was placed in an electrolyte containing 70 wt% phosphoric acid, 2.5 wt% sulfuric acid and 9 wt% chromic acid having a specific gravity of 1.740 kg / l and an iron content of 2.5 wt% at an electrolyte temperature of 50 ° C, a current density of 40 A / dm 2 and a voltage of 11 V eiektropoliert for a period of 6 min.
  • the parts were then rinsed with water and dried.
  • the result of the electropolishing was equivalent in both methods with respect to leveling of the surfaces and smoothing of the cutting edges.
  • Heat-treated steel plates were electropolished in the cured and uncured state in electrolytes according to Example 1.
  • the current density was 25 A / dm 2 at 14 V and an electropolishing time of 60 min.
  • the rinsing process was carried out as described in Example 1, as well as drying in air.
  • the results obtained on the cured and uncured plates were equivalent in terms of material removal, gloss and leveling in both processes.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • ing And Chemical Polishing (AREA)

Claims (10)

  1. Procédé de polissage électrochimique d'aciers faiblement alliés en utilisant un électrolyte qui contient de 100 à 30 % en poids d'acide phosphorique et de 0 à 70 % en poids d'acide sulfurique et dans lequel l'électrolyte est éliminé par rinçage, caractérisé en ce que l'on utilise pour le rinçage une solution contenant de l'acide phosphorique dont la teneur en acide phosphorique est d'au moins 50 % en poids.
  2. Procédé selon la revendication 1, caractérisé en ce que l'on utilise pour le rinçage de l'acide phosphorique concentré.
  3. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte est sensiblement exempt de chrome.
  4. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte présente une teneur en eau maximale de 20 % en poids.
  5. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte contient de 80 à 50 % en poids d'acide phosphorique et de 20 à 50 % en poids d'acide sulfurique.
  6. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte contient des ions fer dans une quantité d'au moins 1 % en poids.
  7. Procédé selon la revendication 6, caractérisé en ce que l'électrolyte présente plus de 2,0 % en poids, mais au maximum environ 8 % en poids d'ions fer.
  8. Procédé selon l'une des revendications précédentes, caractérisé en ce qu'après le rinçage avec la solution contenant de l'acide phosphorique, l'acier poli par voie électrochimique est rincé à l'eau.
  9. Procédé selon la revendication 8, caractérisé en ce que les acides minéraux contenus dans l'eau de rinçage sont récupérés.
  10. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte est complété au moins en partie par l'acide phosphorique enrichi en électrolyte provenant de la première étape de rinçage et, le cas échéant, par de l'acide phosphorique récupéré d'au moins une autre étape de rinçage à l'eau.
EP06776534.7A 2005-08-09 2006-07-31 Procede d'electropolissage Not-in-force EP1913181B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005037563A DE102005037563B3 (de) 2005-08-09 2005-08-09 Elektropolierverfahren
PCT/EP2006/007583 WO2007017156A1 (fr) 2005-08-09 2006-07-31 Procede d'electropolissage

Publications (2)

Publication Number Publication Date
EP1913181A1 EP1913181A1 (fr) 2008-04-23
EP1913181B1 true EP1913181B1 (fr) 2017-10-04

Family

ID=36973892

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06776534.7A Not-in-force EP1913181B1 (fr) 2005-08-09 2006-07-31 Procede d'electropolissage

Country Status (6)

Country Link
US (1) US20090200178A1 (fr)
EP (1) EP1913181B1 (fr)
JP (1) JP2009504905A (fr)
DE (1) DE102005037563B3 (fr)
HU (1) HUE037490T2 (fr)
WO (1) WO2007017156A1 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007011632B3 (de) * 2007-03-09 2008-06-26 Poligrat Gmbh Elektropolierverfahren für Titan
DE102012104707A1 (de) * 2012-05-31 2013-12-05 Benteler Automobiltechnik Gmbh Verfahren zum Herstellen eines Abgaswärmetauschers
US9504554B2 (en) * 2013-01-16 2016-11-29 Biotronik Ag Microstructured absorbable implant
US9163322B2 (en) * 2013-07-01 2015-10-20 General Electric Company Method and apparatus for refurbishing turbine components
US10557212B2 (en) 2016-03-08 2020-02-11 Chemeon Surface Technology, Llc Electropolishing method and product

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB601980A (en) * 1944-04-20 1948-05-18 Westinghouse Electric Int Co Improved process for removing burrs, slivers and fine metal particles from ferrous laminations
BE494931A (fr) * 1949-04-07
US2740755A (en) * 1953-04-01 1956-04-03 Dwight E Couch Electropolishing with phosphorous acid
US2773821A (en) * 1956-06-12 1956-12-11 Electro Gleam Inc Composition for use in electropolishing
GB835594A (en) * 1957-03-15 1960-05-25 Samuel Fox And Company Ltd Improved method and means for the treatment of wire
US4306946A (en) * 1980-08-18 1981-12-22 General Electric Company Process for acid recovery from waste water
EP0249650B1 (fr) * 1986-06-20 1989-12-13 Poligrat Gmbh Electrolyte pour le polissage électrochimique de surfaces de métaux
EP1443129A1 (fr) * 2003-01-30 2004-08-04 Mir-Chem GmbH Procédé d'usinage d'une pièce métallique

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Also Published As

Publication number Publication date
DE102005037563B3 (de) 2006-09-28
WO2007017156A1 (fr) 2007-02-15
JP2009504905A (ja) 2009-02-05
US20090200178A1 (en) 2009-08-13
HUE037490T2 (hu) 2018-08-28
EP1913181A1 (fr) 2008-04-23

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