EP0175598B1 - Verfahren zur Vorbehandlung von Oberflächen aus Uran oder Uranlegierungen - Google Patents

Verfahren zur Vorbehandlung von Oberflächen aus Uran oder Uranlegierungen Download PDF

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Publication number
EP0175598B1
EP0175598B1 EP85401419A EP85401419A EP0175598B1 EP 0175598 B1 EP0175598 B1 EP 0175598B1 EP 85401419 A EP85401419 A EP 85401419A EP 85401419 A EP85401419 A EP 85401419A EP 0175598 B1 EP0175598 B1 EP 0175598B1
Authority
EP
European Patent Office
Prior art keywords
uranium
solution
pickling
process according
rinsing
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.)
Expired
Application number
EP85401419A
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English (en)
French (fr)
Other versions
EP0175598A1 (de
Inventor
Michel Anzola
Daniel Lefevre
Patrick Massicot
Jacques Pierre
Antoine Henry
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.)
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Original Assignee
Commissariat a lEnergie Atomique CEA
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.)
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Publication date
Application filed by Commissariat a lEnergie Atomique CEA filed Critical Commissariat a lEnergie Atomique CEA
Publication of EP0175598A1 publication Critical patent/EP0175598A1/de
Application granted granted Critical
Publication of EP0175598B1 publication Critical patent/EP0175598B1/de
Expired legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/46—Pretreatment of metallic surfaces to be electroplated of actinides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
    • C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
    • C23C18/1837—Multistep pretreatment
    • C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/30—Acidic compositions for etching other metallic material

Definitions

  • the subject of the present invention is a process for the preparation of the surface of uranium or uranium-based alloy parts, carried out with a view to producing nickel plating on these parts by chemical nickel plating.
  • French patent application FR-A-2 017 505 describes chemical solutions for etching uranium which are formed from an aqueous solution of ferric chloride or from a mixture of ferric chloride and nickel chloride. These solutions provide more uniform etching of the exposed surfaces of uranium compared to conventional solutions containing nickel chloride and nitric acid.
  • the present invention specifically relates to a method of preparing the surface of a part made of uranium or uranium alloy, which precisely makes it possible to obtain a good surface condition over the whole of the part.
  • the method according to the invention is characterized in that it comprises a step of chemical attack on the surface of the part made of uranium or of uranium alloy by means of a solution comprising only nickel chloride and hydrochloric acid.
  • an attack solution constituted by a solution of nickel chloride NiCI 2 and hydrochloric acid makes it possible to obtain improved results compared to those obtained with the solutions of the prior art, in particular the solutions described in French patent 1,564,575.
  • an attack is obtained slower than with the CuCl 2 solution, fine and regular, which makes it possible to obtain a satisfactory surface finish on the entire part, even when it is of complicated shape.
  • the attack is not too fast and, therefore, easily controllable.
  • the thickness attacked as a function of time is linear.
  • the use of such solutions also proves to be advantageous since they practically do not change over time and therefore have good storage stability.
  • the nickel chloride NiCI 2 concentration in the solution is 600 to 700 g ⁇ l- 1 and the hydrochloric acid concentration in the solution is 1.8 to 2.2 mol ⁇ l -1 .
  • an aqueous solution containing approximately 615 g ⁇ l -1 of NiCI 2 and approximately 2 mol ⁇ l -1 of HCl can be used as the attack solution.
  • this chemical attack is carried out at ambient temperature for a period of 5 to 10 min.
  • the aqueous solution used for this etching step comprises only nickel chloride, hydrochloric acid and 1.5 to 5.6 mol.I-1 of hydrofluoric acid.
  • the pickling (s) with the sodium hydroxide solution are preferably carried out hot, for example at a temperature of 75 ° C.
  • the operations of pickling with the nitric acid solution are carried out at room temperature using a solution containing 7 to 9 mol ⁇ l -1 of nitric acid, for example an 8 mol solution ⁇ l -1 nitric acid, for periods ranging from 8 to 15 min.
  • the operation is generally carried out at a temperature of 70 to 85 ° C, and a solution containing 250 to 350 g ⁇ l -1 of sodium hydroxide is used; the duration of this pickling can vary from 3 to 7 min.
  • the uranium or uranium alloy parts treated by the process of the invention can then be coated with nickel by chemical nickel plating in aqueous solution.
  • NIPOSIT 65 solutions sold by the company SHIPLEY S.A. are used.
  • the attack is carried out using an aqueous solution containing 615 g ⁇ l -1 of NiCI 2 and 1.99 mol ⁇ l -1 of hydrochloric acid for the durations varying from 0.5 to 10 min ., and we measure the thickness attacked in each case.
  • the value of Ra is also determined (in ⁇ m).
  • the results obtained are given in the table (1) which follows and in the appended figure which represents the attacked thickness (in ⁇ m) as a function of the duration of the chemical etching step (in min.).
  • the intercept difference indicates that the uranium-vanadium alloy attacks slowly during the preliminary stripping steps. If hydrofluoric acid is added to the etching solution, the etching speed is reduced, but the etched thickness always increases linearly as a function of time.
  • etching solution is used as in Examples 1 to 7 for different durations, then a nickel coating is deposited on the parts, using a commercially available solution: NIPOSIT 65.
  • Nickel deposition adhesion tests are then carried out on a Quad Tester Coating adhesion machine, that is to say by means of pins bonded to the coating and then pulled.
  • the same etching solution was used as in Examples 1 to 7 and the etching was carried out for a time such that the etched thickness was 30 ⁇ m.
  • the parts were then covered with a nickel coating 30 ⁇ m thick (eg 29) and 60 ⁇ m thick (eg 30) by chemical nickel plating in a Shipley NiP65 bath.
  • the uranium or uranium alloy parts made of depleted uranium, then treated by the process of the invention and then coated with nickel by chemical nickel plating can thus be used as shielding or ballasting parts in a marine atmosphere.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Chemically Coating (AREA)
  • ing And Chemical Polishing (AREA)

Claims (12)

1. Verfahren zur Vorbehandlung der Oberfläche eines Teils aus Uranium oder einer Uraniumlegierung, dadurch gekennzeichnet, daß es den schritt eines chemischen Angriffs an der Oberfläche des Teils aus Uranium oder Uraniumlegierung mittels einer wässrigen Lösung umfaßt, die ausschließlich Nickelchlorid und Salzsäure umfaßt.
2. Verfahren zur Vorbehandlung der Oberfläche eines Teils aus Uranium oder einer Uraniumlegierung, dadurch gekennzeichnet, daß es den Schritt eines chemischen Angriffs an der Oberfläche des Teils aus Uranium oder einer Uraniumlegierung mittels einer wässrigen Lösung umfaßt, die ausschließlich Nickelchlorid, Salzsäure und 1,5 bis 5,6 mol.I-1 Fluoruasserstoffsäure umfaßt.
3. Verfahren nach irgendeinem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß die Nickelchloridkonzentration der Lösung 600 bis 700 g·l-1 beträgt.
4. Verfahren nach irgendeinem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Salzsäurekonzentration der Lösung 1,8 bis 2,2 mol·l-1 beträgt.
5. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Lösung zum Angriff ungefähr 615 g.I-1 NiCI2 und ungefähr 2 mol·l-1 HCI enthält.
6. Verfahren nach irgendeinem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß der chemische Angriff bei der Umgebungstemperatur während einer Dauer von 5 bis 10 min. durchgeführt wird.
7. Verfahren nach irgendeinem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß man vor der Durchführung dieses chemischen Angriffsschrittes den Teil aus Uranium oder Uraniumlegierung venigstens einer der folgenden Behandlungen aussetzt:
- Entfettung mit einem organischen Lösungsmittel,
- Sandstrahlen,
- Beizen in einer Sodalösung, und
- Beizen in einer Salpetersäurelösung.
8. Verfahren nach irgendeinem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß man nach der chemischen Angriffsstufe den Teil Venigstens einer der folgenden Behandlungen aussetzt:
- Beizen mit einer Salpetersäurelösung, und
- Beizen mit einer Sodalösung.
9. Verfahren nach irgendeinem der Ansprüche 7 oder 8, dadurch gekennzeichnet, daß der oder die Beizvorgänge mit der Sodalösung bei Wärme durchgeführt wird bzw. verden.
10. Verfahren nach irgendeinem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß es die folgenden aufeinanderfolgenden Schritte umfaßt:
- Entfettung mit einem organischen Lösungsmittel,
- feuchtes Sandstrahlen,
- Beizen mit einer Sodalösung in Wärme mit folgendem Waschen mit Wasser,
- Beizen mit einer Salpetersäurelösung mit folgendem Waschen mit Wasser,
- chemischer Angriff mit der Lösung von Nickelchlorid NiCI2 und Salzsäure mit folgendem Waschen mit Wasser,
- Beizen mit einer Salpetersäurelosung mit folgendem Waschen mit Wasser,
- Beizen mit einer Sodalösung in Wärme mit folgendem Waschen mit Wasser, und
- Beizen mit einer Salpetersäurelösung mit folgendem Waschen mit Wasser.
11. Verfahren zum Aufbringen eines Nickelüberzugs auf die Oberfläche eines Teils aus Uranium oder einer Uraniumlegierung, dadurch gekennzeichnet, daß es darin besteht, den Teil aus Uranium oder einer Uraniumlegierung einem Verfahren der Oberflächenvorbehandlung gemäß irgendeinem der Ansprüche 1 bis 10 auszusetzen und daraufhin auf den derart behandelten Teil einen Nickelüberzug durch chemische Vernickelung aufzubringen.
12. Verfahren nach irgendeinem der Ansprüche 1 bis 11, dadurch gekennzeichnet, daß der Teil aus einer Uran-Vanadium-Legierung ist.
EP85401419A 1984-07-18 1985-07-11 Verfahren zur Vorbehandlung von Oberflächen aus Uran oder Uranlegierungen Expired EP0175598B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8411387 1984-07-18
FR8411387A FR2567913B1 (fr) 1984-07-18 1984-07-18 Procede de preparation de la surface de pieces en uranium ou en alliage a base d'uranium

Publications (2)

Publication Number Publication Date
EP0175598A1 EP0175598A1 (de) 1986-03-26
EP0175598B1 true EP0175598B1 (de) 1988-09-21

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EP85401419A Expired EP0175598B1 (de) 1984-07-18 1985-07-11 Verfahren zur Vorbehandlung von Oberflächen aus Uran oder Uranlegierungen

Country Status (4)

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US (1) US4673585A (de)
EP (1) EP0175598B1 (de)
DE (1) DE3565126D1 (de)
FR (1) FR2567913B1 (de)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2590275B1 (fr) * 1985-11-19 1992-07-17 Commissariat Energie Atomique Procede de preparation de la surface d'une piece en alliage d'uranium et de titane, notamment en vue d'un nickelage chimique
TW214570B (de) * 1989-06-30 1993-10-11 Eltech Systems Corp

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB853522A (en) * 1945-01-09 1960-11-09 Atomic Energy Authority Uk Nickel coatings and method of applying
US2928168A (en) * 1945-01-24 1960-03-15 Allen G Gray Iron coated uranium and its production
BE559886A (de) * 1956-08-08
US2984884A (en) * 1958-06-09 1961-05-23 Aerpat Ag Stressed panel fastener
FR1564575A (de) * 1968-01-24 1969-04-25
US3573120A (en) * 1968-09-06 1971-03-30 Atomic Energy Commission Uranium etchant and method
US3700482A (en) * 1970-12-01 1972-10-24 Atomic Energy Commission Uranium surface preparation for electroless nickel plating

Also Published As

Publication number Publication date
DE3565126D1 (en) 1988-10-27
EP0175598A1 (de) 1986-03-26
FR2567913B1 (fr) 1989-11-10
US4673585A (en) 1987-06-16
FR2567913A1 (fr) 1986-01-24

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