US2734837A - Surface treatment of titanium or - Google Patents
Surface treatment of titanium or Download PDFInfo
- Publication number
- US2734837A US2734837A US45871054A US2734837A US 2734837 A US2734837 A US 2734837A US 45871054 A US45871054 A US 45871054A US 2734837 A US2734837 A US 2734837A
- Authority
- US
- United States
- Prior art keywords
- titanium
- surface treatment
- hydrochloric acid
- treatment
- articles
- 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 - Lifetime
Links
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 19
- 239000010936 titanium Substances 0.000 title claims description 19
- 229910052719 titanium Inorganic materials 0.000 title claims description 19
- 238000004381 surface treatment Methods 0.000 title claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000001464 adherent effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 229960002050 hydrofluoric acid Drugs 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000010622 cold drawing Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 229940098221 silver cyanide Drugs 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BAKALPNAEUOCDL-UHFFFAOYSA-N titanium hydrochloride Chemical compound Cl.[Ti] BAKALPNAEUOCDL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05B—CONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
- G05B19/00—Programme-control systems
- G05B19/02—Programme-control systems electric
- G05B19/18—Numerical control [NC], i.e. automatically operating machines, in particular machine tools, e.g. in a manufacturing environment, so as to execute positioning, movement or co-ordinated operations by means of programme data in numerical form
- G05B19/408—Numerical control [NC], i.e. automatically operating machines, in particular machine tools, e.g. in a manufacturing environment, so as to execute positioning, movement or co-ordinated operations by means of programme data in numerical form characterised by data handling or data format, e.g. reading, buffering or conversion of data
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03M—CODING; DECODING; CODE CONVERSION IN GENERAL
- H03M1/00—Analogue/digital conversion; Digital/analogue conversion
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03M—CODING; DECODING; CODE CONVERSION IN GENERAL
- H03M1/00—Analogue/digital conversion; Digital/analogue conversion
- H03M1/12—Analogue/digital converters
- H03M1/22—Analogue/digital converters pattern-reading type
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T409/00—Gear cutting, milling, or planing
- Y10T409/30—Milling
- Y10T409/30084—Milling with regulation of operation by templet, card, or other replaceable information supply
Definitions
- This invention relates to the treatment of titanium or titanium base alloy articles for the purpose of preparing an activated surface thereon prior to for example electroplating.
- Titanium on exposure to air or other oxidising atmospheres forms a surface skin consisting chiefly of oxide, the complete removal of which to give a surface capable of receiving a good electrodeposited coating of another metal is not readily effected by standard pickling or etching compositions.
- the treatment with the hydrochloric acid is effected at 90-100 C.
- the time of treatment depends upon the surface condition of the articles, thus at 90-100" C. it may vary from 5 to 15 minutes.
- a standard pickling solution for example hydrofluoric acid/nitric acid solution
- a standard caustic melt descaling bath consisting of molten sodium hydroxide with or without the addition of other constituents, before treatment with the hydrochloric acid.
- titanium rods to be silver-plated were immersed for 5-15 minutes in boiling commercial hydrochloric acid contained in an electrically heated glass vessel. They were then washed in hot water, rinsed in cold water, and thereupon transferred immediately to a standard plating bath containing silver nitrate, cyanide and potassium carbonate.
- the method of the invention is particularly useful for the pretreatment of titanium surfaces which are to be electroplated, but it may also be used with advantage in cases Where an adherent coating of a metal is required to be applied by methods other than electrodeposition.
- Method of surface treatment of titanium or titanium base alloy articles prior to deposition of a coating metal thereon which comprises treating the surface of the said articles with concentrated hydrochloric acid solution at a temperature between C. and the boiling point of said solution.
- Method in accordance with temperature is 90100 C.
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Human Computer Interaction (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Automation & Control Theory (AREA)
- Theoretical Computer Science (AREA)
- Keying Circuit Devices (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Electroplating Methods And Accessories (AREA)
Description
United States Patent SURFACE TREATMENT OF TITANIUM OR TITANIUM BASE ALLOYS Sidney Hands, Walsall, England, assignor to Chemical Industries Limited, poration of Great Britain N 0 Drawing. Application September 27, 1954, Serial No. 458,710
Imperial London, England, a cor- This invention relates to the treatment of titanium or titanium base alloy articles for the purpose of preparing an activated surface thereon prior to for example electroplating.
Titanium on exposure to air or other oxidising atmospheres forms a surface skin consisting chiefly of oxide, the complete removal of which to give a surface capable of receiving a good electrodeposited coating of another metal is not readily effected by standard pickling or etching compositions.
According to the present invention we provide a method of surface treatment of titanium or titanium base alloy articles prior to deposition of a coating metal thereon which comprises treating the surface of the said articles with concentrated hydrochloric acid solution at elevated temperature.
Preferably the treatment with the hydrochloric acid is effected at 90-100 C. The time of treatment depends upon the surface condition of the articles, thus at 90-100" C. it may vary from 5 to 15 minutes.
Under certain circumstances, for example in the case of heavily scaled material, it may be desirable to pretreat the article with a standard pickling solution, for example hydrofluoric acid/nitric acid solution, or with a standard caustic melt descaling bath consisting of molten sodium hydroxide with or without the addition of other constituents, before treatment with the hydrochloric acid.
By way of example, titanium rods to be silver-plated were immersed for 5-15 minutes in boiling commercial hydrochloric acid contained in an electrically heated glass vessel. They were then washed in hot water, rinsed in cold water, and thereupon transferred immediately to a standard plating bath containing silver nitrate, cyanide and potassium carbonate.
The method of the invention is particularly useful for the pretreatment of titanium surfaces which are to be electroplated, but it may also be used with advantage in cases Where an adherent coating of a metal is required to be applied by methods other than electrodeposition.
One application in which use of the method in accordance with the invention is of considerable benefit is in the cold drawing of titanium or titanium base alloy rod and wire. The effect of the high coeflicient of friction between titanium and the die materials can be overcome by plating the titanium with a metal having a lower coefiicient of friction as a lubricant-retaining layer, but with the electroplates obtainable on titanium by hitherto available methods it has been difiicult or impossible to obtain a degree of adhesion of the coating that would permit high speed drawing to thin gauges. However after preliminary pickling in boiling concentrated hydrochloric acid titanium rod can be plated with a suitable metal from conventional plating baths to give firmly adherent coatings enabling the drawing of fine gauge wire with greater ease and at far higher speed than hitherto possible.
I claim:
1. Method of surface treatment of titanium or titanium base alloy articles prior to deposition of a coating metal thereon, which comprises treating the surface of the said articles with concentrated hydrochloric acid solution at a temperature between C. and the boiling point of said solution.
2. Method in accordance with temperature is 90100 C.
3. Method in accordance with claim 1 in which the article is pretreated with a pickling bath of hydro-fluoric acid/nitric acid solution before treatment with the hydrochloric acid.
4. Method in accordance with claim 1 in which the article is pretreated with a descaling bath of molten sodium hydroxide before treatment with the hydrochloric acid.
5. Method in accordance with claim 1 in which the time of treatment is between 5 and 15 minutes.
potassium claim 1, in which the References Cited in the file of this patent UNITED STATES PATENTS 2,697,051 Mellgren Dec. 14, 1954
Claims (1)
1. METHOD OF SURFACE TREATMENT OF TITANIUM OF TITANIUM BASE ALLOY ARTICLES PRIOR TO DEPOSITION OF A COATING METAL THEREON, WHICH COMPRISES TREATING THE SURFACE OF THE SAID ARTICLES WITH CONCENTRATED HYDROCHLORIC ACID SOLUTION AT A TEMPERATURE BETWEEN 90* C. AND THE BOILING POINT OF SAID SOLUTION
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB336483X | 1953-10-03 | ||
| GB27794/53A GB758013A (en) | 1953-10-03 | 1954-09-22 | Improvements in or relating to the surface treatment of titanium or titanium base alloys |
| GB220954X | 1954-09-22 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2734837A true US2734837A (en) | 1956-02-14 |
Family
ID=27258088
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US45871054 Expired - Lifetime US2734837A (en) | 1953-10-03 | 1954-09-27 | Surface treatment of titanium or |
| US459794A Expired - Lifetime US2949600A (en) | 1953-10-03 | 1954-10-01 | Automatic control systems, especially for automatic machine tools |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US459794A Expired - Lifetime US2949600A (en) | 1953-10-03 | 1954-10-01 | Automatic control systems, especially for automatic machine tools |
Country Status (5)
| Country | Link |
|---|---|
| US (2) | US2734837A (en) |
| BE (1) | BE532416A (en) |
| CH (2) | CH328094A (en) |
| FR (2) | FR1114432A (en) |
| GB (2) | GB796993A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2829091A (en) * | 1956-06-04 | 1958-04-01 | Menasco Mfg Company | Method for electroplating titanium |
| US2856333A (en) * | 1955-06-28 | 1958-10-14 | Tiarco Corp | Electroplating |
| US2938841A (en) * | 1956-04-13 | 1960-05-31 | Olin Mathieson | Preparation of zirconium for cold working |
| US2974021A (en) * | 1957-02-08 | 1961-03-07 | Borowik Albert | Process and composition for chemically treating titanium and its alloys |
| US3007780A (en) * | 1958-03-20 | 1961-11-07 | Titanium Metals Corp | Titanium etching |
| US3278404A (en) * | 1957-07-17 | 1966-10-11 | Ici Ltd | Method and apparatus for cathodic protection |
| US3297552A (en) * | 1963-02-25 | 1967-01-10 | Gisser Henry | Method of making a titanium piece having good anti-wear, anti-galling, antiseizure and anti-friction properties |
| US4804422A (en) * | 1986-02-06 | 1989-02-14 | U.S. Philips Corporation | Method of purifying quartz sand |
| US5660640A (en) * | 1995-06-16 | 1997-08-26 | Joray Corporation | Method of removing sputter deposition from components of vacuum deposition equipment |
| US6261637B1 (en) * | 1995-12-15 | 2001-07-17 | Enthone-Omi, Inc. | Use of palladium immersion deposition to selectively initiate electroless plating on Ti and W alloys for wafer fabrication |
| US6884542B1 (en) * | 2002-05-13 | 2005-04-26 | Zinc Matrix Power, Inc. | Method for treating titanium to electroplating |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB871941A (en) * | 1959-04-17 | 1961-07-05 | Ici Ltd | Improvements in or relating to the surface treatment of titanium or titanium base alloy |
| US3208040A (en) * | 1961-03-14 | 1965-09-21 | Powers & Eaton Ind Inc | Line-casting machine |
| US3246315A (en) * | 1961-10-06 | 1966-04-12 | Ibm | Read only memory |
| US3278810A (en) * | 1963-02-26 | 1966-10-11 | Gen Electric | Relay switching circuit utilizing an enabling voltage source |
| AT278106B (en) * | 1968-02-09 | 1970-01-26 | Siemens Ag | Switching matrix with threshold switch |
| US3641326A (en) * | 1968-11-22 | 1972-02-08 | Buhr Machine Tool Co | Circuit for and method of multiplexing for monitoring a plurality of separate machine tools |
| JPS5916443B2 (en) * | 1976-02-06 | 1984-04-16 | ソニー株式会社 | power amplifier |
| JPS56153832A (en) * | 1980-04-30 | 1981-11-28 | Nec Corp | Digital to analog converter |
| US4322254A (en) * | 1980-09-22 | 1982-03-30 | Uop Inc. | Regeneration of electrical conductivity of metallic surfaces |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2697051A (en) * | 1952-09-17 | 1954-12-14 | Nat Lead Co | Treatment of titanium metal surfaces |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE647724C (en) * | 1937-07-10 | Siemens & Halske Akt Ges | Signaling device with on and reset from the transmitter | |
| US584463A (en) * | 1897-06-15 | Electric signal | ||
| US2682814A (en) * | 1948-01-14 | 1954-07-06 | Graphic Arts Res Foundation In | Photocomposing apparatus |
| US2696600A (en) * | 1950-11-30 | 1954-12-07 | Rca Corp | Combinatorial information-storage network |
| US2685084A (en) * | 1951-04-03 | 1954-07-27 | Us Army | Digital decoder |
| US2738504A (en) * | 1951-08-18 | 1956-03-13 | Gen Precision Lab Inc | Digital number converter |
| US2676289A (en) * | 1951-11-02 | 1954-04-20 | Collins Radio Co | Shaft positioning mechanism for binary code operation |
-
1953
- 1953-10-03 GB GB27178/53A patent/GB796993A/en not_active Expired
-
1954
- 1954-09-22 GB GB27794/53A patent/GB758013A/en not_active Expired
- 1954-09-27 US US45871054 patent/US2734837A/en not_active Expired - Lifetime
- 1954-09-28 CH CH328094D patent/CH328094A/en unknown
- 1954-09-30 CH CH336483D patent/CH336483A/en unknown
- 1954-10-01 US US459794A patent/US2949600A/en not_active Expired - Lifetime
- 1954-10-02 FR FR1114432D patent/FR1114432A/en not_active Expired
- 1954-10-08 BE BE532416D patent/BE532416A/xx unknown
- 1954-10-09 FR FR1109701D patent/FR1109701A/en not_active Expired
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2697051A (en) * | 1952-09-17 | 1954-12-14 | Nat Lead Co | Treatment of titanium metal surfaces |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2856333A (en) * | 1955-06-28 | 1958-10-14 | Tiarco Corp | Electroplating |
| US2938841A (en) * | 1956-04-13 | 1960-05-31 | Olin Mathieson | Preparation of zirconium for cold working |
| US2829091A (en) * | 1956-06-04 | 1958-04-01 | Menasco Mfg Company | Method for electroplating titanium |
| US2974021A (en) * | 1957-02-08 | 1961-03-07 | Borowik Albert | Process and composition for chemically treating titanium and its alloys |
| US3278404A (en) * | 1957-07-17 | 1966-10-11 | Ici Ltd | Method and apparatus for cathodic protection |
| US3007780A (en) * | 1958-03-20 | 1961-11-07 | Titanium Metals Corp | Titanium etching |
| US3297552A (en) * | 1963-02-25 | 1967-01-10 | Gisser Henry | Method of making a titanium piece having good anti-wear, anti-galling, antiseizure and anti-friction properties |
| US4804422A (en) * | 1986-02-06 | 1989-02-14 | U.S. Philips Corporation | Method of purifying quartz sand |
| US5660640A (en) * | 1995-06-16 | 1997-08-26 | Joray Corporation | Method of removing sputter deposition from components of vacuum deposition equipment |
| US6261637B1 (en) * | 1995-12-15 | 2001-07-17 | Enthone-Omi, Inc. | Use of palladium immersion deposition to selectively initiate electroless plating on Ti and W alloys for wafer fabrication |
| US6884542B1 (en) * | 2002-05-13 | 2005-04-26 | Zinc Matrix Power, Inc. | Method for treating titanium to electroplating |
Also Published As
| Publication number | Publication date |
|---|---|
| US2949600A (en) | 1960-08-16 |
| BE532416A (en) | 1958-02-14 |
| GB758013A (en) | 1956-09-26 |
| GB796993A (en) | 1958-06-25 |
| FR1114432A (en) | 1956-04-12 |
| FR1109701A (en) | 1956-02-01 |
| CH328094A (en) | 1958-02-28 |
| CH336483A (en) | 1959-02-28 |
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