US3753875A - Method of treatment of metallic surfaces - Google Patents
Method of treatment of metallic surfaces Download PDFInfo
- Publication number
- US3753875A US3753875A US00151478A US3753875DA US3753875A US 3753875 A US3753875 A US 3753875A US 00151478 A US00151478 A US 00151478A US 3753875D A US3753875D A US 3753875DA US 3753875 A US3753875 A US 3753875A
- Authority
- US
- United States
- Prior art keywords
- bath
- water
- temperature
- treatment
- mixture
- 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
- 238000000034 method Methods 0.000 title abstract description 13
- 150000003839 salts Chemical class 0.000 abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 27
- 239000000203 mixture Substances 0.000 abstract description 19
- 238000009835 boiling Methods 0.000 abstract description 6
- 239000000460 chlorine Substances 0.000 abstract description 6
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 4
- 239000005864 Sulphur Substances 0.000 abstract description 4
- 229910052785 arsenic Inorganic materials 0.000 abstract description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052794 bromium Inorganic materials 0.000 abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 abstract description 4
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052714 tellurium Inorganic materials 0.000 abstract description 4
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 abstract description 4
- 150000003567 thiocyanates Chemical class 0.000 abstract description 2
- -1 SLENIUM Chemical compound 0.000 abstract 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 abstract 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 abstract 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 abstract 1
- 150000003568 thioethers Chemical class 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 239000011669 selenium Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 3
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- OKIIEJOIXGHUKX-UHFFFAOYSA-L cadmium iodide Chemical compound [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 2
- 229940116357 potassium thiocyanate Drugs 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- UDHXJZHVNHGCEC-UHFFFAOYSA-N Chlorophacinone Chemical compound C1=CC(Cl)=CC=C1C(C=1C=CC=CC=1)C(=O)C1C(=O)C2=CC=CC=C2C1=O UDHXJZHVNHGCEC-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000000573 anti-seizure effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940075417 cadmium iodide Drugs 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- 229910052720 vanadium Inorganic materials 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
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/06—Electrolytic coating other than with metals with inorganic materials by anodic processes
Definitions
- a method of treatment of metallic surfaces in order to improve their resistance to wear and to seizure consists of electrolyzing a part having a metallic surface which serves as an anode in a bath consisting of water and one or a. mixture of salts containing at least one element belonging to the group of elements constituted by sulphur, selenium, tellurium, phosphorus, boron, silicon, fluorine, chlorine, iodine, bromine, arsenic, the temperature of the bath being comprised between the ambient temperature and the boiling temperature of the mixture of salt or salts and water.
- the bath may be composed of a mixture of water with alkaline sulphides, thiocyanates or iodides.
- Methods of treatment of metallic surfaces have already been proposed for the purpose of improving their qualities of friction and resistance to wear, these methods consisting of introducing a non-metal into the metallic surface treated by electrolysis in a bath of molten salts, the part to be treated being anodic, that is to say connected to the positive pole of a current supply source, the bath being at a temperature at least equal to the melting temperature of the salts.
- the parts treated by these known methods may have an excellent resistance to wear and to seizure, but there are cases in which the treatment temperature is incompatible with certain mechanical or physical characteristics of the parts to be treated.
- certain hardened steels are utilized after tempering at a temperature lower than 150 C. If it is desired to sulphurize these steels in a bath having a base of potassium thiocyanate, the temperature of the bath must be chosen to be higher than this value; in this case, the treatment results in a reduction of the hardness.
- the formation of cadmium iodide at the surface of a part of cadmium from a bath of salts with a base of sodium iodide can be obtained by electrolysis in a bath at a temperature at least equal to the melting point of this salt, namely 665 C. At this temperature the cadmium is in fusion and this results in a degradation of the surface condition of the parts.
- the present invention has for its object a method for carrying out at very low temperatures the treatment of metallic surfaces by the introduction of a non-metal into the superficial layers.
- the method according to the invention consists of electrolyzing a part having a metallic surface and acting as an anode in a bath composed of water and a salt or a mixture of salts containing at least one element which belongs to the group of elements constituted by sulphur, selenium, tellurium, phosphorus, boron, silicon, fluorine, chlorine, iodine, bromine, arsenic, the temperature of the bath being comprised between the ambient temperature and the boiling point of the mixture of salts plus water.
- water is added to the anhydrous salt in a proportion such that the quantity of salt (or mixture of salts) present in the water is 3,753,875 Patented Aug. 21, 1973 at least equal to the limit of solubility of the said salt or mixture of salts.
- the mixture thus made is brought up to a temperature at most equal to its boiling temperature, and the initial quantity of water is maintained in the bath by an appropriate means which effects a continuous or discontinuous addition of water.
- the part in which the surface to be treated is immersed in the bath thus made is subjected to electrolysis in the bath by being connected to the positive pole of a current supply source, at a current density comprised between 0.1 and 30 amperes per sq. dm., for a period comprised between 1 and 60 minutes.
- a layer with a base of one or a number of compounds between the metal forming the part itself and one or a number of the anion and/or cation elements added by the salt or the mixture of salts for example iron sulphide and double iron sulphide and sodium sulphide in the case where a steel part is treated in a bath consisting of a mixture of water and sodium sulphide.
- This layer which is perfectly adherent to the base metal, gives the treated parts excellent anti-seizure and anti-wear properties.
- This heat treatment has a purpose of increasing the surface hardness by dilfusion of the non-metal towards the interior of the part, while forming a hardness gradient which decreases from the surface towards the interior of the said part.
- EXAMPLE 1 The part to be treated is made of nickel.
- the bath employed is composed of of a salt or mixture of salts containing at least one of the elements: sulphur, selenium, tellurium, phosphorus, boron, silicon, fluorine, chlorine, iodine, bromine, arsenic, and 20% of water.
- This salt or mixture of salts may comprise in particular an alkaline sulphide or thiocyanate or iodide.
- the bath utilized is composed of:
- the quantity of salt present in the Water is at least equal to the limit of solubility of this salt in water.
- the time of treatment is comprised between 0.1 and 60 minutes and is preferably equal to 15 minutes.
- the direct current density is comprised between 0.1 and 30 amperes per sq. dm. and is preferably equal to 0.6 A. per sq. dm.
- the part to be treated plays the part of an anode.
- the treatment temperature is comprised between ambient temperature and the boiling temperature of the mixture of salt plus water and is more particularly maintained at 110 C.
- the slow evaporation of the water initially contained in the bath is compensated by a continuous addition of water at the rate of 30 cu. cm. per hour and per litre of mixture.
- EXAMPLE 2 The part to be treated is of 16 NC 6 steel, case hardened and tempered (having a composition of 011% C, 0.3% Si, 0.8% Mn, 1% Cr, 1.25% Ni, the remainder iron).
- the bath employed is composed of:
- the temperature of the bath is maintained at 130 C.
- the bath is kept homogeneous by gaseous agitation.
- the metal crucible containing the bath is used as a cathode, and the test sample is placed at the anode.
- the directcurrent density is 5 a. per sq. dm.
- the slow evaporation of the water initially contained in the bath is compensated by an addition of water at a rate of 45 cu. cm. per hour and per litre of mixture.
- the Faville friction test gave the following figures: whereas a test sample of 16 NC 6 case-hardened, tempered, ground and not treated seizes-up during the first seconds of the test, the test sample treated under the above conditions creeps without seizure after 75 seconds operation when the gripping load of the jaws on the test sample is 5,500N.
- EXAMPLE 3 The part to be treated is in this case a cylindrical test piece of 6.5 mm. in diameter, and 40 mm. in height, in titanium alloy TA6V (Afnor Standard), having the composition: 0.07% C, 0.22% Fe, 6.24% Al, 3.93% V, 0.30% impurities, the remainder being titanium.
- the electrolytic bath is a solution of potassium iodide dissolved in water to saturation and brought up to a temperature of 115 C.
- test piece is heat treated in a non-reactive atmosphere at a temperature comprised between 115 C. and 850 C. and preferably at a temperature of 800 C.
- Micrographic examination of this test piece brings into evidence a layer of 340 microns in thickness, the hardness of which passes, as a result of a diffusion of titanium iodide into the alloy, from 1,000 HV at the surface to 457 HV at 250 microns (the hardness in the heart of the test piece being 344 HV, that is to say that of the untreated TA6V).
- a method of treating metallic surfaces so as to improve their resistance to Wear and to seizure comprising electrolyzing a part having a surface of a metal selected from the group consisting of iron, nickel and titanium, as an anode in a bath consisting essentially of water and at least one salt whose cation is selected from the group consisting of sodium and potassium and whose anion is selected from the group consisting of sulphide, thiocyanate and iodide, at a temperature between ambient temperature and the boiling temperature of the bath,
- the electrolyzing current being direct current of 0.1 to 30 amperes per square decimeter and the duration of said electrolysis being 0.1 to minutes.
Landscapes
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Heat Treatment Of Articles (AREA)
- Chemical Treatment Of Metals (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Lubricants (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR7023726A FR2092874B1 (enrdf_load_stackoverflow) | 1970-06-26 | 1970-06-26 | |
| FR7103716A FR2124083B2 (enrdf_load_stackoverflow) | 1970-06-26 | 1971-02-04 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3753875A true US3753875A (en) | 1973-08-21 |
Family
ID=26215818
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00151478A Expired - Lifetime US3753875A (en) | 1970-06-26 | 1971-06-09 | Method of treatment of metallic surfaces |
Country Status (10)
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4452675A (en) * | 1982-10-18 | 1984-06-05 | Allied Corporation | Process for the activation of nickel electrodes via the electrochemical deposition of selenium and/or tellurium |
-
1970
- 1970-06-26 FR FR7023726A patent/FR2092874B1/fr not_active Expired
-
1971
- 1971-02-04 FR FR7103716A patent/FR2124083B2/fr not_active Expired
- 1971-06-09 US US00151478A patent/US3753875A/en not_active Expired - Lifetime
- 1971-06-10 BE BE768350A patent/BE768350A/xx unknown
- 1971-06-22 NL NL7108562A patent/NL7108562A/xx not_active Application Discontinuation
- 1971-06-23 DE DE2131152A patent/DE2131152C3/de not_active Expired
- 1971-06-24 GB GB2969271A patent/GB1338791A/en not_active Expired
- 1971-06-25 CH CH936771A patent/CH527913A/fr not_active IP Right Cessation
- 1971-06-25 ES ES392619A patent/ES392619A1/es not_active Expired
- 1971-06-25 CA CA116,732A patent/CA957640A/en not_active Expired
- 1971-06-25 CS CS7100004727A patent/CS180574B2/cs unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4452675A (en) * | 1982-10-18 | 1984-06-05 | Allied Corporation | Process for the activation of nickel electrodes via the electrochemical deposition of selenium and/or tellurium |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2124083B2 (enrdf_load_stackoverflow) | 1975-06-06 |
| DE2131152C3 (de) | 1980-08-21 |
| CS180574B2 (en) | 1978-01-31 |
| NL7108562A (enrdf_load_stackoverflow) | 1971-12-28 |
| FR2092874A1 (enrdf_load_stackoverflow) | 1972-01-28 |
| FR2124083A2 (enrdf_load_stackoverflow) | 1972-09-22 |
| ES392619A1 (es) | 1973-08-16 |
| CA957640A (en) | 1974-11-12 |
| DE2131152A1 (de) | 1971-12-30 |
| DE2131152B2 (de) | 1979-12-20 |
| GB1338791A (en) | 1973-11-28 |
| CH527913A (fr) | 1972-09-15 |
| BE768350A (fr) | 1971-11-03 |
| FR2092874B1 (enrdf_load_stackoverflow) | 1973-10-19 |
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