US3369914A - Method of chemically polishing iron, zinc and alloys thereof - Google Patents
Method of chemically polishing iron, zinc and alloys thereof Download PDFInfo
- Publication number
- US3369914A US3369914A US410378A US41037864A US3369914A US 3369914 A US3369914 A US 3369914A US 410378 A US410378 A US 410378A US 41037864 A US41037864 A US 41037864A US 3369914 A US3369914 A US 3369914A
- Authority
- US
- United States
- Prior art keywords
- alloys
- iron
- hydrogen fluoride
- zinc
- solution
- 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title description 22
- 229910045601 alloy Inorganic materials 0.000 title description 17
- 239000000956 alloy Substances 0.000 title description 17
- 238000005498 polishing Methods 0.000 title description 14
- 229910052742 iron Inorganic materials 0.000 title description 11
- 238000000034 method Methods 0.000 title description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title description 9
- 229910052725 zinc Inorganic materials 0.000 title description 9
- 239000011701 zinc Substances 0.000 title description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 36
- 229910052751 metal Inorganic materials 0.000 description 23
- 239000002184 metal Substances 0.000 description 23
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 21
- 239000000243 solution Substances 0.000 description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 150000002739 metals Chemical class 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- KGWWEXORQXHJJQ-UHFFFAOYSA-N [Fe].[Co].[Ni] Chemical compound [Fe].[Co].[Ni] KGWWEXORQXHJJQ-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910000640 Fe alloy Inorganic materials 0.000 description 3
- 238000007517 polishing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000003892 tartrate salts Chemical class 0.000 description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- -1 for example Chemical compound 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910001092 metal group alloy 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
- 239000000758 substrate Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
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
- 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
-
- 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
- the surface of a metal on which a metal coating is to be deposited by reduction, exchange or electro deposition must have a suitable surface condition in order that the deposition is effected under favourable conditions.
- the shining appearance of the metal surface is an indication that the surface condition is particularly suitable for providing such deposits.
- this condition is met, the adherence of the deposited metal is improved and the metal surface obtained by the deposition, which itself is shining, presents a great resistance against corrosion.
- the solderability of such thin films which are deposited on a shining substrate is better than that of the films which are deposited on a dull metal.
- the shining appearance of a metal surface is a criterion for the resistance against corrosion and may be used to obtain decorative effects.
- a method of electrolytically polishing zinc by means of acid or basic solutions in an oxidizing medium is known as well as that for obtaining a polished surface of titanium, zirconium and alloys thereof by means of a mixture containing hydrogen fluoride.
- the chemical polishing may be difficult if not impossible.
- the various metals and alloys do not behave in the same manner with respect to the same acid solution. If, in addition, the various alloys are welded to one assembly, this remains electrochemically heterogeneous and the difference in tension at the contact places between the various components as a rule involves a preferred chemical attack.
- the method of chemically polishing according to the invention is particularly suitable for homogeneous components of iron, nickel or cobalt and also in the case that components of the same metals are combined heterogeneously.
- the invention for applying the invention to the polishing of other alloys it is suflicient to vary the ratios of the composing parts of the polishing bath by adding, if desired, additives suitable for the purpose in view.
- the invention may be applied in particular to carbon steels and may be used for zinc.
- the method of polishing the surface of metals or oxidizable metal alloys, and in particular zinc or analogous metals is characterized in that the surface to be polished is immersed for a restricted period of time in an aqueous solution of hydrogen fluoride and hydrogen peroxide.
- the treatment of the metal surfaces takes place in the cold or in the heat, the optimum temperature for polishing being higher for metals which are less oxidizable and being determined for each individual case. Also the concentration of hydrogen peroxide is proportionally larger according as the metal or the alloy to be polished is less oxidizable.
- the concentration of hydrogen fluoride may be rather weak so that the polishing operation with solution according to the invention can take place in a glass container or in a container which comprises a glass window through which the polishing process can be followed
- the ratio of molecular concentration of hy drogen peroxide-hydrogen fluoride lies between 3 and 7.
- the figure in the drawing shows how the shine of the surface of an alloy varies as a function of the ratio of the concentration of hydrogen peroxide and of hydrogen fluoride.
- the starting products of the solution are concentrated and given the dilution which best corresponds to the metal to be polished.
- These products may consist of a solution of 48 to 50% by weight of hydrogen fluoride, i.e. containing approximately 25 g. mol. of hydrogen fluoride per litre, and a solution of hydrogen peroxide of 30%.
- iron, nickel, cobalt are polished at a temperature of the order of 80 C.
- Ironnickel-cobalt alloys and iron-nickel alloys are polished at a temperature of approximately C,
- the components to be polished are transferred to the container with the solution according to the invention only when the temperature of the latter has been reached and heating has been stopped.
- Example First a solution of hydrogen fluoride is prepared by diluting 210 ml. of the starting solution of hydrogen fluoride 48 to 50% to 1 litre by deionized water. 300 ml. of this solution are added to 1 litre of the starting solution of hydrogen peroxide of 30%.
- the resulting mixture is then diluted with deionized water, for example with 1300 ml., and heated to a temperature of approximately C. in the polishing container which preferably consists of glass. Then heating is discontinued and the components to be polished, for example, components of iron, nickel, cobalt or an alloy of these metals, is immersed in this bath for 1 minute.
- the quality of the resulting polish depends upon the ratio of the concentrations of hydrogen peroxide and hydrogen fluoride and it has been found, that for polishing iron, nickel, cobalt and alloys of iron-nickel a maximum shine is obtained for a molecular ratio of hydrogen peroxide to hydrogen fluoride which is approximately 5 which is the case noticeably with the said solution in the example.
- the shine Br or reflection power of the polished surface varies indeed as a function of the ratio of the concentrations of hydrogen peroxide and hydrogen fluoride.
- the maximum shine is obtained for a volume ratio V V of the above components which equals 3 which corresponds to a molecular ratio of 5.
- the polishing operation is preferably carried out with solutions in which the volume ratio of hydrogen peroxide to hydrogen fluoride lies between 2 and 4 which corresponds to values 3.1 and 6.3 of the molecular ratio.
- the action of the solution on the component to be polished is stronger on the projecting points of the surface where the catalytic decomposition of the hydrogen peroxide is greater. This increased oxidation also involves an increased action of the acid.
- the concentration of hydrogen fluoride is only approximately 1% so that this involves no risks in operation.
- articles consisting of iron or iron alloys for example, iron-nickel-cobalt or iron-nickel, must be treated at elevated temperature. Polishing certain metal component parts for electronic devices sometimes involves difficulties. Some component parts are melted to glass component parts which, when treated with a warm mixture of hydrogen fluoride with hydrogen peroxide, are attacked. The gas-tight and vacuum-tight properties of such a seal which are of great importance for an electronic device, may be adversely influenced by it.
- iron alloys for example, iron-nickel and iron-nickel-cobalt
- a polishing treatment at room temperature namely by a suitable pretreatment of the surface to be polished before it is immersed in the aqueous mixture of hydrogen peroxide and hydrogen fluoride.
- This pretreatment consists in that the articles are kept immersed for a restricted period of time in a mixture of chlorides and tartrates, at an elevated temperature which lies below the boiling point of the solution.
- An exampleof such a pretreatment bath consists of a solution which contains per litre: 300 g. of tartaric acid and 6 mol of hydrochloric acid. This bath is preferably heated at a temperature of approximately 60 C. The time of treatment is approximately 6 to 8 minutes.
- a method of polishing the surface of a metal object selected from the group consisting of iron, zinc and oxidizable alloys thereof said method comprising immersing said metal object for a short period of time in an aqueous solution of hydrogen peroxide and hydrogen fluoride, the molecular ratio of hydrogen peroxide to hydrogen fluoride being between about 3:1 and 7:1.
- metal objects are oxidizable iron alloys selected from the group consistting of nickel-iron and nickel-iron-cobalt alloys.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR953317A FR1383066A (fr) | 1963-11-12 | 1963-11-12 | Procédé de polissage chimique de métaux |
FR970684A FR85595E (fr) | 1964-04-13 | 1964-04-13 | Procédé de polissage chimique de métaux |
Publications (1)
Publication Number | Publication Date |
---|---|
US3369914A true US3369914A (en) | 1968-02-20 |
Family
ID=26204268
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US410378A Expired - Lifetime US3369914A (en) | 1963-11-12 | 1964-11-12 | Method of chemically polishing iron, zinc and alloys thereof |
Country Status (7)
Country | Link |
---|---|
US (1) | US3369914A (en)) |
BE (1) | BE655566A (en)) |
CH (1) | CH450103A (en)) |
DE (1) | DE1270355B (en)) |
GB (1) | GB1056670A (en)) |
NL (1) | NL6413002A (en)) |
OA (1) | OA01154A (en)) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3537926A (en) * | 1967-06-19 | 1970-11-03 | Lancy Lab | Chemical brightening of iron-containing surfaces of workpieces |
US5477976A (en) * | 1990-11-27 | 1995-12-26 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Brightening chemical polishing solution for hardened steel article and method of chemically polishing said article in the solution |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1070189B1 (en) | 1999-02-04 | 2006-06-21 | The Stanley Works | Automatic door assembly and door operator therefor |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2689785A (en) * | 1953-03-18 | 1954-09-21 | Us Navy | Method for chemically polishing lead |
US3103733A (en) * | 1958-08-19 | 1963-09-17 | Clevite Corp | Treatment of germanium semiconductor devices |
US3158517A (en) * | 1959-11-05 | 1964-11-24 | Telefunken Gmbh | Process for forming recesses in semiconductor bodies |
US3228816A (en) * | 1962-02-21 | 1966-01-11 | Rohr Corp | Process and composition for cleaning and polishing aluminum and its alloys |
US3269881A (en) * | 1963-12-30 | 1966-08-30 | Allied Chem | Hydrogen peroxide etching of copper in manufacture of printed circuits |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE710733C (de) * | 1937-10-16 | 1941-09-19 | Schering Ag | Verfahren zum Beizen von Eisen und Eisenlegierungen |
-
0
- BE BE655566D patent/BE655566A/xx unknown
-
1964
- 1964-11-07 NL NL6413002A patent/NL6413002A/xx unknown
- 1964-11-09 CH CH1444064A patent/CH450103A/de unknown
- 1964-11-09 GB GB45575/64A patent/GB1056670A/en not_active Expired
- 1964-11-10 DE DEP1270A patent/DE1270355B/de active Pending
- 1964-11-12 US US410378A patent/US3369914A/en not_active Expired - Lifetime
- 1964-12-31 OA OA51313A patent/OA01154A/xx unknown
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2689785A (en) * | 1953-03-18 | 1954-09-21 | Us Navy | Method for chemically polishing lead |
US3103733A (en) * | 1958-08-19 | 1963-09-17 | Clevite Corp | Treatment of germanium semiconductor devices |
US3158517A (en) * | 1959-11-05 | 1964-11-24 | Telefunken Gmbh | Process for forming recesses in semiconductor bodies |
US3228816A (en) * | 1962-02-21 | 1966-01-11 | Rohr Corp | Process and composition for cleaning and polishing aluminum and its alloys |
US3269881A (en) * | 1963-12-30 | 1966-08-30 | Allied Chem | Hydrogen peroxide etching of copper in manufacture of printed circuits |
US3293093A (en) * | 1963-12-30 | 1966-12-20 | Allied Chem | Dissolution of metal with acidified hydrogen peroxide and use as copper etchant in manufacture of printed circuits |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3537926A (en) * | 1967-06-19 | 1970-11-03 | Lancy Lab | Chemical brightening of iron-containing surfaces of workpieces |
US5477976A (en) * | 1990-11-27 | 1995-12-26 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Brightening chemical polishing solution for hardened steel article and method of chemically polishing said article in the solution |
Also Published As
Publication number | Publication date |
---|---|
OA01154A (fr) | 1968-08-07 |
CH450103A (de) | 1968-01-15 |
BE655566A (en)) | |
DE1270355B (de) | 1968-06-12 |
NL6413002A (en)) | 1965-05-13 |
GB1056670A (en) | 1967-01-25 |
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