US3753815A - Method and bath for treating titanium - Google Patents
Method and bath for treating titanium Download PDFInfo
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- US3753815A US3753815A US00182847A US3753815DA US3753815A US 3753815 A US3753815 A US 3753815A US 00182847 A US00182847 A US 00182847A US 3753815D A US3753815D A US 3753815DA US 3753815 A US3753815 A US 3753815A
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- United States
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- percent
- volume
- bath
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- hydrofluoric acid
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Classifications
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- 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
- C23F1/26—Acidic compositions for etching refractory metals
-
- 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
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
Definitions
- ABSTRACT Primary Examiner-Jacob H. Steinberg Attorney-John Howard Joynt [57] ABSTRACT Method of treating titanium and titanium alloys, especially hot-worked products such as bar, rod, wire and various flat-rolled forms so as to remove seams, fissures and the like, as well as a desired amount of surface metal.
- the products are immersed in a bath comprising some 5 percent to 15 percent by volume hydrofluoric acid, with remainder phosphoric .acid and water, maintained at such temperature and for such time as to re move a desired quantity of metal and yield a dull, satinlike finish free of pitting and ready for further processing.
- the products may be subjected to a preliminary treatment in a molten salt bath, such as sodium hydroxide, and washed in water, this to best condition the products for metal removal.
- Our invention may be considered to consist in the combination of ingredients forming the bath employed, in the several operational steps resorted to and in the relation of each of the same to one or more of the others, all as more especially described herein.
- the scope of the invention is set out in the claims at the end of this specification.
- unalloyed titanium as well as alloyed titanium
- the unalloyed titanium is available in various grades with mechanical properties ranging from a tensile strength of some 35,500 psi and elongation of about 25 percent on up to strengths on the order of 80,000 psi tensile, with elongations on the order of percent.
- the unalloyed titanium is fusio n-weldable and is available in the forms of weld rod and weld wire for welding various titanium alloys.
- titanium alloys As to the titanium alloys, tensile strength on the order of some 130,000 psi with yield of 120,000 psi and elongation of 10 percent characterizes a typical alphabeta-alloy analyzing about 6 percent aluminum, about 4 percent vanadium with remainder titanium. The alloy is characterized by good corrosion resistance along with strength as noted. A further alpha-beta titanium alloy of somewhat greater strength contains about 6 percent aluminum, 6 percent vanadium, 2 percent tin, with remainder titanium. This alloy enjoys good welding and fabricating characteristics.
- a titanium alloy which is especially suited for coldheading applications contains about 11.5 percent molybdenum, 6 percent zirconium, 4.5 percent tin, with remainder titanium. This is the Beta III alloy and is available in the form of bar and billet, sheet, strip and other fiat-rolled products, as well as wire. It is readily weldable.
- the surface imperfections extend beneath the surface a distance of some 2 to 10 mils, that is, some 0.002 inches to some 0.010 inches. And that, with the removal of surface metal in accordance with the teachings of our invention, these imperfections are either eliminated or so minimized, as by rounding off the edges or flattening out the depressions, that with further processing, e.g., cold-rolling, cold-drawing or the like, a uniform surface free of physical blemish is effectively achieved.
- the surface metal is removed by employing a bath essentially consisting of hydrofluoric and phosphoric acids in aqueous solution.
- a bath essentially consisting of hydrofluoric and phosphoric acids in aqueous solution.
- chlorides there is an absence of chlorides.
- the amount of phosphoric acid may vary over a fairly broad range of concentration, the amount of hydrofluoric acid employed is most critical.
- Phosphoric acid is used in the amount of about 5 percent to about 25 percent by volume of concentrated acid (85 percent by weight), this ordinarily amounting to some 5 percent to 15 percent by volume.
- the amount of concentrated (48 percent by weight) hydrofluoric acid employed is limited to some 5 percent to 15 percent by volume, especially some 7 percent to 15 percent or even 10 percent to percent. In all instances, the remainder of the bath is principally water.
- the amount of hydrofluoric acid employed is most critical, for with a hydrofluoric acid content less than 5 percent by volume, hydrogen absorption becomes excessive.
- the concentration of the bath should be at least 7 percent by volume hydrofluoric acid.
- the hydrofluoric acid should be present in the amount of about 10 percent by volume.
- the time of treatment in the bath ranges from some five minutes to some 25 minutes, this, of course, depending upon hydrofluoric acid concentration and bath temperature, as well as the amount of metal to be removed.
- the metal Upon withdrawing the products from the bath, the metal is washed with water under pressure and set aside to dry. Scams and fissures are seen to have been opened up and dished out. We find the surface to be of dull, satin-like quality. There is no pitting. And there is no polish.
- titanium products When desired, as where significant oxide film is present as a result of prior mill treatment, we first subject the titanium products to a preliminary or conditioning treatment in a molten salt bath. Molten sodium hydroxide with addition of oxidizing salts is conveniently used, following which the products are washed in water in readiness for further treatment.
- the method of treating titanium and titanium alloys in accordance with our inven tion contemplates immersion in a bath comprising hydrofluoric acid in the amount of about 5 percent to 15 percent by volume, phosphoric acid in the amount of about 5 percent to about 25 percent by volume, with remainder substantially all water, as set out above, a best combination of results is had with particular amounts of the hydrofluoric and phosphoric acids. Andalthough the temperature of the bath may vary somewhat, that is, between about some F. up to some 145 F., we feel that best results in matters of metal removal consistent with a minimum of hydrogen absorption is had where the bath is maintained at a tempera ture of some to F.
- the time of treatment generally depends upon the hydrofluoric acid concentration and upon bath temperature. Within the broad ranges indicated of the bath composition and temperature, time of treatment usually ranges from some two minutes to 20 minutes.
- a preferred method in accordance with the teachings of our invention employs a bath comprising about 10 percent by volume hydrofluoric acid and 10 percent by volume phosphoric acid with remainder water.
- the bath is maintained at a temperature of about 120 F. to about 140 F., although satisfactory results are had where the temperature is as low as 1 15 F. A temperature exceeding F., however, is not acceptable because the speed of the reaction between metal and bath becomes difficult to control and because of excessive hydrogen absorption.
- metal is removed from the surface at the rate of about one-half mil per minute. Hydrogen absorption amounts to about 1 part per million for each mil removed from the surface of the metal. Treatment for about 20 minutes results in the removal of about 10 mils from the surface.
- a further preferred method and bath comprises about 7 percent to 10 percent by volume hydrofluoric acid and about 5 percent to 15 percent by volume phosphoric acid.
- the remainder of the composition is water.
- a desired quantity of metal is removed in a matter of 15 or 20 minutes time.
- the rate of removal is on the order of one-half mil per minute. Edges of seams and fissures are rounded off.
- a dull satin finish is had with freedom from pitting and freedom from polish.
- the surface is readily conditioned to accept a suitable lubricant, soap, lead or the like, for further treatment, that is, cold-drawing, extruding or the like.
- a further preferred method and bath comprises about 10 percent to 15 percent by volume hydrofluoric acid and about 5 percent to about 15 percent phosphoric acid or, more broadly, about 5 percent to 25 percent by volume phosphoric acid, with remainder water. With the bath temperature maintained at some 120 to 140 F., metal is removed from the surface at the rate of about one-half mil per minute. Because of the high concentration of hydrofluoric acid, hydrogen absorption is at a minimum. There is achieved in a matter of minutes a surface of dull satin finish suited to the application of lubricant and further processing.
- samples of the titanium-6 percent aluminum-4 percent vanadium alloy in form of 0.206 inch diameter wire we treated in a bath consisting of about 10 percent by volume phosphoric acid and with hydrofluoric acid in the amounts of one-half percent, 3 percent, 5 percent, 7 percent and 10 percent by volume.
- the bath was maintained at a temperature of about 120 F.
- Samples also were treated with the bath temperature maintained at 140 F.
- the time of the treatment was 1 hour.
- the wires of each coil were moved about on the yoke, so as to expose surfaces previously in contact with each other, and the coils then further immersed in the bath for an additional period of time. After another 4 minutes in the bath, the coils were withdrawn and a check made of the further metal loss. With removal of the desired amount of metal, a total of about 10 mils off the diameter, the coils were washed down with water under pressure and then set aside to dry.
- the temperature of the bath may be maintained relatively constant, as from about 130 to 140 F., by means of refrigerating equipment.
- refrigerating equipment employs a vat for containing the bath in which refrigerating tubing is embedded in the side walls thereof.
- titanium phosphate precipitates out in the form of titanium phosphate.
- about 3 pounds of titanium phosphate sludge accumulates at the bottom of the bath for every pound of titanium removed from the metal being treated.
- This sludge for effective bath life, is removed by scooping it out from time to time.
- suitable filtering equipment or suitable centrifuge equipment may be employed for sludge removal. With the removal of sludge, the necessity for bath replacement is effectively minimized.
- For effective bath life not only are there required additions of hydrofluoric acid from time to time, as noted, but also there are required additions of phosphoric acid, this to compensate for the loss by the formation of the titanium phosphate precipitated.
- the coils treated in accordance with our invention when dried following treatment and wash, reveal a surface of satin-like quality, free of pitting.
- the amount of metal removed from the surface is found to be uniform throughout the product. Hair cracks and fissures either are eliminated or are so flattened out, with edges rounded off, as to give a smooth, crack-free surface upon further processing, as by cold-drawing, for example.
- Method of chemically removing metal from hotworked titanium products such as bar, rod, wire which comprises subjecting the same to molten sodium hydroxide; washing in water; and then subjecting to a solution essentially consisting of about 5 percent to percent by volume hydrofluoric acid with remainder phosphoric acid in amount not exceeding about percent by volume, and water at least about 60 percent by volume.
- Method of chemically removing metal from hotworked titanium products such as bar, rod, wire which comprises subjecting the same to molten sodium hydroxide; washing in water; and then subjecting to a solution essentially consisting of about 5 percent to 15 percent by volume of hydrofluoric acid, about 5 percent to about 25 percent by volume of phosphoric acid, and water at least about 60 percent by volume.
- the method of chemically removing metal from the surface of titanium products which comprises treating the products in a bath essentially consisting of about 5 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water at least about 60 percent by volume while maintaining the bath at a temperature of at least about F. but not exceeding about 145 F.
- the method of chemically removing hairlines, surface cracks, fissures and surface metal generally from titanium products which comprises treating the products in an aqueous bath essentially consisting of about 10 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 15 percent by volume phosphoric acid, and water at least about 60 percent by volume while maintaining the bath at a temperature of about F. to about F. for such time as to remove a desired quantity of metal and give a surface of dull satin finish without either pitting or polish.
- the method of chemically removing hairlines, surface cracks, tissures and surface metal generally from titanium products which comprises treating the products in an aqueous bath essentially consisting of about 7 percent to about 10 percent by volume hydrofluoric acid, about 5 percent to about 15 percent by volume phosphoric acid, and water at least about 60 percent by volume while the bath is maintained at a temperature of about 120 to 140 F. and for such time as to give a surface of dull satin finish without pitting or polish.
- the method of chemically removing metal from the surface of titanium products with maximum rate of metal removal consistent with minimum hydrogen absorption comprises treating the products in an aqueous bath essentially consisting of about 10 percent by volume hydrofluoric acid and about 10 percent by volume phosphoric acid, and water at least about 60 percent by volume while maintaining the bath at a temperature of about 120 F. to about 140 F.
- the method of chemically removing metal from the surface of titanium products which comprises treating the products in an aqueous bath essentially consisting of about 5 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water at least about 60 percent by volume; maintaining the bath at a temperature of about 120 to about 140 F.; and when the rate of metal removal has slowed to a value less than about 0.5 mils per minute spiking the bath with hydrofluoric acid.
- the method of chemically removing metal from the surface of titanium products which comprises treating the products in an aqueous bath essentially consisting of about 5 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water at least about 60 percent by volume while the bath is maintained at a temperature of about 120 F. to about 140 F. to achieve a surface of dull satin finish without pit or polish; and when the rate of metal removal falls below about 0.5 mils per minute, removing sludge from the bottom of the bath and spiking the same with hydrofluoric acid in the amount of about 2 percent to about 15 percent by volume.
- a bath for chemically removing metal from titanium products essentially consisting of about 5 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water in the amount of at least 60 percent by volume.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Description
Claims (8)
- 2. Method of chemically removing metal from hot-worked titanium products such as bar, rod, wire which comprises subjecting the same to molten sodium hydRoxide; washing in water; and then subjecting to a solution essentially consisting of about 5 percent to 15 percent by volume of hydrofluoric acid, about 5 percent to about 25 percent by volume of phosphoric acid, and water at least about 60 percent by volume.
- 3. The method of chemically removing metal from the surface of titanium products which comprises treating the products in a bath essentially consisting of about 5 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water at least about 60 percent by volume while maintaining the bath at a temperature of at least about 115* F. but not exceeding about 145* F.
- 4. The method of chemically removing hairlines, surface cracks, fissures and surface metal generally from titanium products which comprises treating the products in an aqueous bath essentially consisting of about 10 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 15 percent by volume phosphoric acid, and water at least about 60 percent by volume while maintaining the bath at a temperature of about 120* F. to about 140* F. for such time as to remove a desired quantity of metal and give a surface of dull satin finish without either pitting or polish.
- 5. The method of chemically removing hairlines, surface cracks, fissures and surface metal generally from titanium products which comprises treating the products in an aqueous bath essentially consisting of about 7 percent to about 10 percent by volume hydrofluoric acid, about 5 percent to about 15 percent by volume phosphoric acid, and water at least about 60 percent by volume while the bath is maintained at a temperature of about 120* to 140* F. and for such time as to give a surface of dull satin finish without pitting or polish.
- 6. The method of chemically removing metal from the surface of titanium products with maximum rate of metal removal consistent with minimum hydrogen absorption which comprises treating the products in an aqueous bath essentially consisting of about 10 percent by volume hydrofluoric acid and about 10 percent by volume phosphoric acid, and water at least about 60 percent by volume while maintaining the bath at a temperature of about 120* F. to about 140* F.
- 7. The method of chemically removing metal from the surface of titanium products which comprises treating the products in an aqueous bath essentially consisting of about 5 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water at least about 60 percent by volume; maintaining the bath at a temperature of about 120* to about 140* F.; and when the rate of metal removal has slowed to a value less than about 0.5 mils per minute spiking the bath with hydrofluoric acid.
- 8. The method of chemically removing metal from the surface of titanium products which comprises treating the products in an aqueous bath essentially consisting of about 5 percent to about 15 percent by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water at least about 60 percent by volume while the bath is maintained at a temperature of about 120* F. to about 140* F. to achieve a surface of dull satin finish without pit or polish; and when the rate of metal removal falls below about 0.5 mils per minute, removing sludge from the bottom of the bath and spiking the same with hydrofluoric acid in the amount of about 2 percent to about 15 percent by volume.
- 9. A bath for chemically removing metal from titanium products essentially consisting of about 5 percent to about 15 percEnt by volume hydrofluoric acid, about 5 percent to about 25 percent by volume phosphoric acid, and water in the amount of at least 60 percent by volume.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US18284771A | 1971-09-22 | 1971-09-22 |
Publications (1)
Publication Number | Publication Date |
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US3753815A true US3753815A (en) | 1973-08-21 |
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US00182847A Expired - Lifetime US3753815A (en) | 1971-09-22 | 1971-09-22 | Method and bath for treating titanium |
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3944496A (en) * | 1973-04-30 | 1976-03-16 | Coggins Dolphus L | Composition for chemical milling refractory metals |
US4944986A (en) * | 1988-09-23 | 1990-07-31 | Zuel Company | Anti-reflective glass surface |
US5102499A (en) * | 1991-01-07 | 1992-04-07 | United Technologies Corporation | Hydrogen embrittlement reduction in chemical milling |
US5120605A (en) * | 1988-09-23 | 1992-06-09 | Zuel Company, Inc. | Anti-reflective glass surface |
US5389194A (en) * | 1993-02-05 | 1995-02-14 | Lsi Logic Corporation | Methods of cleaning semiconductor substrates after polishing |
WO2000066808A1 (en) * | 1999-04-30 | 2000-11-09 | Yury Vyacheslavovich Kislyakov | Method for chemically processing articles made of titanium or alloys thereof |
US20050099337A1 (en) * | 2003-11-12 | 2005-05-12 | Hitachi, Ltd. | Antenna, method for manufacturing the antenna, and communication apparatus including the antenna |
US6929861B2 (en) | 2002-03-05 | 2005-08-16 | Zuel Company, Inc. | Anti-reflective glass surface with improved cleanability |
US20080169270A1 (en) * | 2007-01-17 | 2008-07-17 | United Technologies Corporation | Method of removing a case layer from a metal alloy |
CN103103550A (en) * | 2013-01-17 | 2013-05-15 | 河南航天精工制造有限公司 | Surface treatment method of titanium and titanium alloys |
US20130299456A1 (en) * | 2012-05-09 | 2013-11-14 | Mitsubishi Heavy Industries, Ltd. | Method of removing work-affected layer |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3383255A (en) * | 1964-11-05 | 1968-05-14 | North American Rockwell | Planar etching of fused silica |
US3562013A (en) * | 1967-10-23 | 1971-02-09 | Diversey Corp | Process of deoxidizing titanium and its alloys |
-
1971
- 1971-09-22 US US00182847A patent/US3753815A/en not_active Expired - Lifetime
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3383255A (en) * | 1964-11-05 | 1968-05-14 | North American Rockwell | Planar etching of fused silica |
US3562013A (en) * | 1967-10-23 | 1971-02-09 | Diversey Corp | Process of deoxidizing titanium and its alloys |
Non-Patent Citations (3)
Title |
---|
Metal Finishing 1 22 70 Guidebook Directory. * |
Pickling and Acid Dipping by Hall pp. 219, 220. * |
Titanium Metals Handbook, pp. 16 and 19. * |
Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3944496A (en) * | 1973-04-30 | 1976-03-16 | Coggins Dolphus L | Composition for chemical milling refractory metals |
US4944986A (en) * | 1988-09-23 | 1990-07-31 | Zuel Company | Anti-reflective glass surface |
US5120605A (en) * | 1988-09-23 | 1992-06-09 | Zuel Company, Inc. | Anti-reflective glass surface |
US5102499A (en) * | 1991-01-07 | 1992-04-07 | United Technologies Corporation | Hydrogen embrittlement reduction in chemical milling |
US5389194A (en) * | 1993-02-05 | 1995-02-14 | Lsi Logic Corporation | Methods of cleaning semiconductor substrates after polishing |
WO2000066808A1 (en) * | 1999-04-30 | 2000-11-09 | Yury Vyacheslavovich Kislyakov | Method for chemically processing articles made of titanium or alloys thereof |
US6929861B2 (en) | 2002-03-05 | 2005-08-16 | Zuel Company, Inc. | Anti-reflective glass surface with improved cleanability |
US20050099337A1 (en) * | 2003-11-12 | 2005-05-12 | Hitachi, Ltd. | Antenna, method for manufacturing the antenna, and communication apparatus including the antenna |
US7015862B2 (en) * | 2003-11-12 | 2006-03-21 | Hitachi, Ltd. | Antenna, method for manufacturing the antenna, and communication apparatus including the antenna |
US20080169270A1 (en) * | 2007-01-17 | 2008-07-17 | United Technologies Corporation | Method of removing a case layer from a metal alloy |
EP1947217A1 (en) * | 2007-01-17 | 2008-07-23 | United Technologies Corporation | Method of removing an alpha-case titanium layer from a beta-phase titanium alloy |
US20130299456A1 (en) * | 2012-05-09 | 2013-11-14 | Mitsubishi Heavy Industries, Ltd. | Method of removing work-affected layer |
US9481934B2 (en) * | 2012-05-09 | 2016-11-01 | Mitsubishi Heavy Industries Aero Engines, Ltd. | Method of removing work-affected layer |
CN103103550A (en) * | 2013-01-17 | 2013-05-15 | 河南航天精工制造有限公司 | Surface treatment method of titanium and titanium alloys |
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