US2865797A - Method of forming carbonaceous protective coatings on titanium and zirconium - Google Patents
Method of forming carbonaceous protective coatings on titanium and zirconium Download PDFInfo
- Publication number
- US2865797A US2865797A US694504A US69450457A US2865797A US 2865797 A US2865797 A US 2865797A US 694504 A US694504 A US 694504A US 69450457 A US69450457 A US 69450457A US 2865797 A US2865797 A US 2865797A
- Authority
- US
- United States
- Prior art keywords
- titanium
- zirconium
- protective coatings
- carbonaceous protective
- forming carbonaceous
- 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 description 8
- 229910052719 titanium Inorganic materials 0.000 title description 8
- 239000010936 titanium Substances 0.000 title description 8
- 238000000034 method Methods 0.000 title description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title description 4
- 229910052726 zirconium Inorganic materials 0.000 title description 4
- 239000011253 protective coating Substances 0.000 title description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 238000000576 coating method Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- NSMXQKNUPPXBRG-SECBINFHSA-N (R)-lisofylline Chemical compound O=C1N(CCCC[C@H](O)C)C(=O)N(C)C2=C1N(C)C=N2 NSMXQKNUPPXBRG-SECBINFHSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/20—Carburising
Definitions
- Claim. (Cl. 148-131) This invention relates to protective coatings on titanium and zirconium and their alloys. It relates particularly to such coatings for protection of the metals and alloys during heat treatment and working.
- the improved method of this invention consists in heating the metal part to be protected in a pure hydrocarbon vapor in a temperature range of 7501000 C.
- the metal in this treatment forms a thin coating of carbide covered with a layer of carbon.
- the metal or alloy treated in this way is protected from oxidation when heated in air to temperatures in the range 750-900 C.
- the hydrocarbon vapor must be free from oxygen, nitrogen or metallic impurities.
- Example I In this example, I take pure titanium containing .025 oxygen; I heat for 30 minutes to 800 C. in an atmosphere of butane, and cool in the gas. I now heat this material in air at 850 C. for 1 hour. For comparison, I take an untreated piece of the same titanium and heat it in air at 850 C. for 1 hour. I then determine the oxygen penetration into the titanium surface in the two pieces. The results follow:
- Example 11 In this example, I take pure zirconium and proceed as in Example I except that I use pure methane at 750 C. in the coating operation. After heating in air at 900 C. for 1 hour, I find that the oxygen penetration in the heated piece is limited to 4 mils, while in the untreated piece oxygen has penetrated for 20 mils.
- Example 111 Example IV In this example, I proceed as in Example I except that the alloy is titanium, 10% aluminum. I heat to 800 C. in pure ethyline for 20 minutes and cool in the gas. I now heat this material in air at 850 C. for 1 hour. I find that oxygen penetration has been limited to a surface zone 3 mils thick.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Description
United htates Patent METHOD OF FORMING CARBONACEOUS PRO- TEC'IIIJVE COATINGS ON TITANIUM AND ZIR- CON M Frank X. McCawley, Cheverly, Md., assignor to Chicago Development Corporation, Riverdale, Md., a corporation of Delaware N 0 Drawing. Application November 5, 1957 Serial No. 694,504
1 Claim. (Cl. 148-131) This invention relates to protective coatings on titanium and zirconium and their alloys. It relates particularly to such coatings for protection of the metals and alloys during heat treatment and working.
In my copending application, Serial No. 668,771, filed June 25, 1957, I have disclosed that carbide coatings are effective means for the protection of titanium alloys at high temperatures. I have disclosed in that application several methods of producing such coatings. The present invention is concerned with improved methods of producing such coatings.
The improved method of this invention consists in heating the metal part to be protected in a pure hydrocarbon vapor in a temperature range of 7501000 C. The metal in this treatment forms a thin coating of carbide covered with a layer of carbon.
The metal or alloy treated in this way is protected from oxidation when heated in air to temperatures in the range 750-900 C. To prevent contamination of the surface, the hydrocarbon vapor must be free from oxygen, nitrogen or metallic impurities.
Having now described my invention in its more general aspects, I will illustrate it by examples.
Example I In this example, I take pure titanium containing .025 oxygen; I heat for 30 minutes to 800 C. in an atmosphere of butane, and cool in the gas. I now heat this material in air at 850 C. for 1 hour. For comparison, I take an untreated piece of the same titanium and heat it in air at 850 C. for 1 hour. I then determine the oxygen penetration into the titanium surface in the two pieces. The results follow:
0; Content Mlle from Surface Coated Uncoated I a .025 .042 a 025 035 m 025 030 12 025 028 14 025 026 16 .025 .025 18 .025 .025 20 025 025 2,865,797 Patented Dec. 23, 1958 It will be seen that the carbide coating restricts oxygen absorption a layer at the surface less than 4 mils thick.
Example 11 In this example, I take pure zirconium and proceed as in Example I except that I use pure methane at 750 C. in the coating operation. After heating in air at 900 C. for 1 hour, I find that the oxygen penetration in the heated piece is limited to 4 mils, while in the untreated piece oxygen has penetrated for 20 mils.
Example 111 Example IV In this example, I proceed as in Example I except that the alloy is titanium, 10% aluminum. I heat to 800 C. in pure ethyline for 20 minutes and cool in the gas. I now heat this material in air at 850 C. for 1 hour. I find that oxygen penetration has been limited to a surface zone 3 mils thick.
What is claimed is:
The method of treating a metal mass selected from the group consisting of titanium, titanium alloys, zirconium and zirconium alloys in an oxidizing atmosphere at 6001100 0., Without oxygen penetration to a depth of more than about 4 mils which consists in first heating in a pure hydrocarbon vapor at 7501000 C. for 10-30 minutes.
References Cited in the file of this patent Hanzel: Metal Progress, March 1954, pages 91, 92. Griest et al.: American Society for Metals Transactions, vol. 46, 1954, page 267.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US694504A US2865797A (en) | 1957-11-05 | 1957-11-05 | Method of forming carbonaceous protective coatings on titanium and zirconium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US694504A US2865797A (en) | 1957-11-05 | 1957-11-05 | Method of forming carbonaceous protective coatings on titanium and zirconium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2865797A true US2865797A (en) | 1958-12-23 |
Family
ID=24789083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US694504A Expired - Lifetime US2865797A (en) | 1957-11-05 | 1957-11-05 | Method of forming carbonaceous protective coatings on titanium and zirconium |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2865797A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3234055A (en) * | 1962-11-06 | 1966-02-08 | Selas Corp Of America | Method of uniformly heating metal pieces |
| US3640597A (en) * | 1964-01-06 | 1972-02-08 | Varian Associates | Method of producing neutron source tube with coated target |
| WO2002053792A1 (en) * | 2000-12-28 | 2002-07-11 | Centro Sviluppo Materiali S.P.A. | Process for the surface treatment of titanium, items made of or coated with titanium and treated according to such process |
-
1957
- 1957-11-05 US US694504A patent/US2865797A/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| None * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3234055A (en) * | 1962-11-06 | 1966-02-08 | Selas Corp Of America | Method of uniformly heating metal pieces |
| US3640597A (en) * | 1964-01-06 | 1972-02-08 | Varian Associates | Method of producing neutron source tube with coated target |
| WO2002053792A1 (en) * | 2000-12-28 | 2002-07-11 | Centro Sviluppo Materiali S.P.A. | Process for the surface treatment of titanium, items made of or coated with titanium and treated according to such process |
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