US2650875A - Method of etching aluminum and aluminum base alloys - Google Patents
Method of etching aluminum and aluminum base alloys Download PDFInfo
- Publication number
- US2650875A US2650875A US200117A US20011750A US2650875A US 2650875 A US2650875 A US 2650875A US 200117 A US200117 A US 200117A US 20011750 A US20011750 A US 20011750A US 2650875 A US2650875 A US 2650875A
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- United States
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- aluminum
- etching
- alkali
- acid
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- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title claims description 32
- 229910052782 aluminium Inorganic materials 0.000 title claims description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 28
- 238000005530 etching Methods 0.000 title claims description 21
- 239000000956 alloy Substances 0.000 title claims description 7
- 229910045601 alloy Inorganic materials 0.000 title claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 16
- 150000007513 acids Chemical class 0.000 claims description 9
- 239000002585 base Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- 230000001464 adherent effect Effects 0.000 claims description 3
- ORXJMBXYSGGCHG-UHFFFAOYSA-N dimethyl 2-methoxypropanedioate Chemical compound COC(=O)C(OC)C(=O)OC ORXJMBXYSGGCHG-UHFFFAOYSA-N 0.000 claims description 2
- CBOIHMRHGLHBPB-UHFFFAOYSA-N hydroxymethyl Chemical compound O[CH2] CBOIHMRHGLHBPB-UHFFFAOYSA-N 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 45
- 239000000243 solution Substances 0.000 description 24
- 239000003513 alkali Substances 0.000 description 18
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 9
- 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 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 239000011734 sodium Substances 0.000 description 9
- 125000001931 aliphatic group Chemical group 0.000 description 7
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 6
- 239000000174 gluconic acid Substances 0.000 description 6
- 235000012208 gluconic acid Nutrition 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000007792 addition Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 244000215068 Acacia senegal Species 0.000 description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 4
- RGHNJXZEOKUKBD-SQOUGZDYSA-M D-gluconate Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O RGHNJXZEOKUKBD-SQOUGZDYSA-M 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 229920000084 Gum arabic Polymers 0.000 description 4
- 239000000205 acacia gum Substances 0.000 description 4
- 235000010489 acacia gum Nutrition 0.000 description 4
- 229940050410 gluconate Drugs 0.000 description 4
- 150000002596 lactones Chemical class 0.000 description 4
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000600 sorbitol Substances 0.000 description 4
- 235000010356 sorbitol Nutrition 0.000 description 4
- 235000000346 sugar Nutrition 0.000 description 4
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 3
- 229920002261 Corn starch Polymers 0.000 description 3
- DSLZVSRJTYRBFB-UHFFFAOYSA-N Galactaric acid Natural products OC(=O)C(O)C(O)C(O)C(O)C(O)=O DSLZVSRJTYRBFB-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- -1 alkali metal salt Chemical class 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000008120 corn starch Substances 0.000 description 3
- DSLZVSRJTYRBFB-DUHBMQHGSA-N galactaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)C(O)=O DSLZVSRJTYRBFB-DUHBMQHGSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000176 sodium gluconate Substances 0.000 description 3
- 235000012207 sodium gluconate Nutrition 0.000 description 3
- 229940005574 sodium gluconate Drugs 0.000 description 3
- 150000005846 sugar alcohols Polymers 0.000 description 3
- 150000008163 sugars Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PHOQVHQSTUBQQK-SQOUGZDYSA-N D-glucono-1,5-lactone Chemical compound OC[C@H]1OC(=O)[C@H](O)[C@@H](O)[C@@H]1O PHOQVHQSTUBQQK-SQOUGZDYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 2
- 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 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000008101 lactose Substances 0.000 description 2
- 239000013014 purified material Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000001124 (E)-prop-1-ene-1,2,3-tricarboxylic acid Substances 0.000 description 1
- BDDLHHRCDSJVKV-UHFFFAOYSA-N 7028-40-2 Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O BDDLHHRCDSJVKV-UHFFFAOYSA-N 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- 101100349264 Caenorhabditis elegans ntr-1 gene Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GXGJIOMUZAGVEH-UHFFFAOYSA-N Chamazulene Chemical group CCC1=CC=C(C)C2=CC=C(C)C2=C1 GXGJIOMUZAGVEH-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- OCUCCJIRFHNWBP-IYEMJOQQSA-L Copper gluconate Chemical class [Cu+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O OCUCCJIRFHNWBP-IYEMJOQQSA-L 0.000 description 1
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
- SHZGCJCMOBCMKK-JFNONXLTSA-N L-rhamnopyranose Chemical compound C[C@@H]1OC(O)[C@H](O)[C@H](O)[C@H]1O SHZGCJCMOBCMKK-JFNONXLTSA-N 0.000 description 1
- PNNNRSAQSRJVSB-UHFFFAOYSA-N L-rhamnose Natural products CC(O)C(O)C(O)C(O)C=O PNNNRSAQSRJVSB-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229940091181 aconitic acid Drugs 0.000 description 1
- IAJILQKETJEXLJ-QTBDOELSSA-N aldehydo-D-glucuronic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-QTBDOELSSA-N 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- GTZCVFVGUGFEME-IWQZZHSRSA-N cis-aconitic acid Chemical compound OC(=O)C\C(C(O)=O)=C\C(O)=O GTZCVFVGUGFEME-IWQZZHSRSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229930182830 galactose Natural products 0.000 description 1
- 235000012209 glucono delta-lactone Nutrition 0.000 description 1
- 229960003681 gluconolactone Drugs 0.000 description 1
- 229940097043 glucuronic acid Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- BALXUFOVQVENIU-KXNXZCPBSA-N pseudoephedrine hydrochloride Chemical compound [H+].[Cl-].CN[C@@H](C)[C@@H](O)C1=CC=CC=C1 BALXUFOVQVENIU-KXNXZCPBSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- 239000002699 waste material Substances 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
- 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
- C23F1/32—Alkaline compositions
- C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
Definitions
- This invention relatestto a. method: of etchin aluminum and aluminum base; aiu ysl.
- the alumina isapparently the principal constituent of the hard-rock-like scale
- thermorethe scale that is formed often adheres.
- etching aluminum and aluminum base 4 as arabinose, rhamnose, galactose and fructose, which is a ketone sugar, starch and gum arabic are useful in controlling precipitation but sometimes excessive foaming occurs with these latter ll y W hout h f rm i n of r ck-like le 5 two materials.
- the most desirable inhibitors are by employing a method wherein the article of gluconic acid, mucic acid, the alkali metal salts aluminum or a u num a y is trea w t a of these acids, glucoheptonic lactone, gluco lachot aqueous solution comprising an etching altone, corn starch, sorbitol and gum arabic.
- Glukali and a small amount of a water soluble satuconic acid or its salts appears to be the most deted aliphatic p y y y inhibitor Compound sirable inhibitor because of its stability in heated described in ea er de l here ters solutions, uniformity of results obtained and new method Operates either by p event ng the commercial availability.
- the gluconic reversion of the sodium aluminate to sod u yacid may be added as such to the etching solution droxide and alum a y controlling this where it is immediately converted to the alkali version so that any scale formed iS in ge metal salt or the alkali metal salt itself may be granular and u non-adherent t0 the su added.
- the gluconic reversion of the sodium aluminate to sod u yacid may be added as such to the etching solution droxide and alum a y controlling this where it is immediately converted to the alkali version so that any scale formed iS in ge metal salt or the alkali metal salt itself may be granular and u non-adherent t0 the su added.
- the polyhydroxy inhibitors coming within the 4.5 1 96 above described class include polyhydric alcohols 2 d 3 Yes having the formula CH20H(CHOH)
- COOH(CHOH) dCOOH regenerated sodium hydroxide two solutions were wherein d is at least 2, and acids having the charged at 8 ounces per gallon in separate steel generaly formula CI-IOICHOHMCOOH wherein e containers heated with steam coils at 160 F.
- A- further advantage obtained in using. a suitable hydroxyv compound as described herein is the. elimination or the substantial reduction of the problems involved. in removing smut often formed during aluminumetching.
- This smut is ordinarily silicon, carbon, copper on. other materials left at. the surface of the article being etched after. removalv of the aluminum by the etching solution.
- The. removal of this smut often requires additional treatment in an acid bath.
- aluminum and. aluminum base" alloys are treated accordingto the method of this invention the smut that remains can be removed much easier so that the removal time is reduced byv /3 to as compared with similar articles etched in a bath according to the old methods.
- the new method leaves the smut in such a condition that it can be easily rinsed off so that the usual acid treatment is unnecessary.
- a preferred composition for use in applicants? method is made up of 96% by' weight of sodium hydroxide and 1% of technical 50% gluconic acid. This acid, of course, is converted immedi-- ately to sodium gluconate.
- the solution is main-- tained at a temperature of from 120 F. to 210 F during the treatment and the polyhydroxy compound is present in an amount of 0.5% to 10% by weight of the combined alkali and the com-- pound.
- the alkali is: present in an amount of 4.0% to 10.0% by weight of the solution.
- the method which comprises treating the surface of said article with a hot aqueous solution comprising an etching alkali and a small amount of water-soluble saturated aliphatic polyhydroxy compound in a proportion such that the formation of a hard adherent precipitate is avoided for an extended period of time, said compound being selected from the class consisting of polyhydric alcohols of the formula CI-IzOI-HCHOHMCHzOH wherein a is at least 2, starches of the formula (C6H10O5)z, polyhydroxy monobasic acids of the formula COOH(CHOH) cCH2OH wherein c is at least 4, polyhydroxy dibasic acids of the formula COOH CHOH COOH wherein (Z is at least 3, gum arabic and the alkali metal salts of said acids.
- a hot aqueous solution comprising an etching alkali and a small amount of water-soluble saturated aliphatic polyhydroxy compound in a proportion such that the formation of a hard adherent precipitate is avoided for an extended period of time
- the method which comprises treating the surface of said article with an aqueous solution containing ounces per gallon of a mixture of 98% by weight of sodium hydroxide and 2% by weight of sodium gluconate while maintaining said solution at a temperature of about to F.
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- 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)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Description
Patented Sept. 1, 1953 METHQD. 015' E'LCHING. ALUMINUM A UM NUM BASE ALLOYS Vladimir Dvorkovitz, Chicago, and John R.. Swihart Ghicago. Heights, 111., assignors to The niverse} Qorporation, a corporation of Illinois Nit-Drawing. Application December 9, 1950,
Serial No. 200,117
11 Claims.
This invention relatestto a. method: of etchin aluminum and aluminum base; aiu ysl.
In many instances. whereartjicles. of: aluminum or aluminum base alloys; are tahrijcated it is, necessary to etch the; surfiace-of. the; article.- either as n id in fabricationofthe article. to provide a e for further finishin -co e give avfinal decorative finish. The. usuat industrial; practice in etching e materials: is to treat-the; surface of the article, with, a, hot; aqueous: soluti n coirta ninsan etch n alkali. such. as sodium hyx d p ssium. hydroxide. trisod um choc: p t s da ash. r s milar-mat r als;- Qrm xtures of these chemicals in varying proportions. Because of the chemical activity of the aluminum, it reacts with these alkaline etching chemicals to form aluminum reaction products as may be represented; by the reaction with sodium hydroxide:
Although such practicesin'the past have been. effective in etching the metals, these methods are not entirely satisfiactor y and the; n'iethod has certain inherent disadyanl figfia Probably the most importantv of thesedisadvanta es is the formation of a, hardrock-like scale. or m ss in the etching tank whichisdeposited on the sides of the tank, on the heating units in the tank and on other surfaces. This scale is ordinarily so hard and tenaciousthat lt is quite, diifiou t to remove. Generally this scale canonly be, re,- moved by chipping it; off with. hammers. or; other tools. This not onlycauses loss, oi. time .andexpensive labor costs but thetb leaking looseof the scale often damages the equipment. The scale is apparently formed. whenthe concentration of, the alkali in theretching solution becomes reduced due to the; reaction oi the alkali with the, metal. When this happensathe: sodiumalumia re ionproduct. reacts with water t P cip tate huninummlirdroxide. accordin o h equation:
The aluminum, hydroxide apparently thenreacts further to precipitate alumina according to the following eq ation:
The alumina, isapparently the principal constituent of the hard-rock-like scale;
It is known that; the scale formation can be postponed for a short period by the addition of fresh alkali such as sodium hydroxide to the solution as the alkali, in the solution is used up. However, as, the concentration of aluminum in the solution. increases, the addition of fresh alkali must be similarly increased in amount until these additions; become so large that they upset the control necessary for the production of av uniformly etched product. Thus the attempt to solve the problem by additions of fresh alkali s not. o m y feasible- As can be noted from the aboveequations, the reaction between the water and the sodium aluminate: regenerates; some sodium, hydroxide. While this is of some advantage; it is more than counteracted by the objectionable scale that is also formed; Furthermore this regeneration of alkali cannot be controlled so that as the work is withdrawn from; the: etching bath the regeneration often occurs in the film adhering to the work so that the increased concentration of alkali produces a non-uniform surface. Fur
thermorethe scale that is formed often adheres.
oz/gal. ozlgal. oz/gal'. of'avail. NaO H Precipitate of NaOH regenerated A1203.3H2O' Freshsolution 10. 6 0. 0 Used solution 1.2 0.0 Used solution, after 92 hour 3.0 1.8 7.1 Used solution, after 8 hours. 6. 1 4. 9 19. 2
1 Slight.
The above-table of examplesis only indicative of the results achieved since the degree of reversionis controlled by temperature, additions of alkali as upkeep, the time of the etching process and other variables.
Applicants have successfully solved the problem of etching aluminum and aluminum base 4 as arabinose, rhamnose, galactose and fructose, which is a ketone sugar, starch and gum arabic are useful in controlling precipitation but sometimes excessive foaming occurs with these latter ll y W hout h f rm i n of r ck-like le 5 two materials. The most desirable inhibitors are by employing a method wherein the article of gluconic acid, mucic acid, the alkali metal salts aluminum or a u num a y is trea w t a of these acids, glucoheptonic lactone, gluco lachot aqueous solution comprising an etching altone, corn starch, sorbitol and gum arabic. Glukali and a small amount of a water soluble satuconic acid or its salts appears to be the most deted aliphatic p y y y inhibitor Compound sirable inhibitor because of its stability in heated described in ea er de l here ters solutions, uniformity of results obtained and new method Operates either by p event ng the commercial availability. If desired, the gluconic reversion of the sodium aluminate to sod u yacid may be added as such to the etching solution droxide and alum a y controlling this where it is immediately converted to the alkali version so that any scale formed iS in ge metal salt or the alkali metal salt itself may be granular and u non-adherent t0 the su added. This is, of course, true of any of the other contac d by e b In this letter instance acids. Glycerine and tartaric acid inhibit scale the alumin p cipi f rms as a lu wh formation but are not preferred as their effectivecan be easily washed away due to its non-adness i of h t d ti herent character. The mechanism by which these organic ma- The advantages of the new method of etching terials function to control the precipitation of aluminum as described herein are nu O alumina is not completely understood. However, Thus the invent o prevents costly damage the improved results of the new method have caused by the former necessity of cleaning the b proven i practicalapplicafions q p t y ppin e scal from this p- Several experiments were made using sodium ment. Furt e O the operetOl 0f the etching gluconate in various amounts and as compared bath can exercise better and closer control over with ntr 1 employing di hydroxide and the process so th t he number of rejects are trisodium phosphate and a second control emp y edu ed- The plant shutdowns necesploying sodium hydroxide alone. In each test sa y for r pa a to r p a e the sp nt t in aluminum was etched at 180 F. in a solution consolutions are kept to an absolute minimum. Also, taining 10 ounces per gallon of the etching chemithe full benefit of the chemicals used in the new cals. After no more aluminum would react with process is obtained as objectionable side reactions the solutions, these solutions were allowed to which tend to reduce the efficiency of the process stand for eighteen hours after which they were are kept to a minimum. Other advantages are examined for the effectiveness of the gluconate in the improvement and uniformity in the quality preventing scale precipitation and adherence. of the work produced and the ease of disposal of The following results were obtained. the solid granular waste when the precipitate occurs. Furthermore, subsequent chemical treatments of the etched surfaces are often much Appeab g g easier than was true when prior etching processes solution 10 oz/gal. pf Mix Perance of Precipiwere used. All of these improvements and adoon'mmmk cent 552 il n vantages increase the economy, efiiciency and tainer ease of operation of the etching process.
The polyhydroxy inhibitors coming within the 4.5 1 96 above described class include polyhydric alcohols 2 d 3 Yes having the formula CH20H(CHOH)|1CH2OH, 95 wherein a is at least 1, starches having the gen- 3 n3 5 eral formula [Cs(H20)5], sugars having the 4 fi 98 general formula CHO(CHOH)tCI-I2OH wherein Z) gagfifj Pfffflj 2 t is at least 3, polyhydroxy monobasic acids having 5 the general formula coomcnoiiiccmon wherein c is at least 4, polyhydroxy dibasic acids having the general formula In order to control scale formation and utilize COOH(CHOH) dCOOH regenerated sodium hydroxide, two solutions were wherein d is at least 2, and acids having the charged at 8 ounces per gallon in separate steel generaly formula CI-IOICHOHMCOOH wherein e containers heated with steam coils at 160 F. is at least 4. Among the preferred inhibitors are Aluminum was dissolved for a period of 240 hours. sorbitol as the polyhydric alcohol, corn starch, 0 This was equivalent to four times the theoretical glucose and lactose as the sugars, gluconic acid amount which would react with the caustic presas the monobasic acid and mucic acid as the dient. At the end of that time, each container was basic acid. The salts or lactones of these subexamined for scale and precipitate. Th followstances may also be used. Similarly, gum arabic ing results were noted,
strliclg Boa-fiilgifloilix Percent AmounlaggPrecipi- Condltloiizi1 t08f Preclpi- 1 IgTTZggIIIIIII: 13g Tank%full. Hard rock-like mass. 2 {Purifiedsodiumglu- 2 }Tank}full Sludge.
conate.
which contains glucuronic acid from the family having the last previously described structural The steam coils in solution 1 were coated with a /2 inch of a hard white crystalline deposit which formula may also be used. Other sugars, such was removed only with difiiculty. No solid residue. was observedson the con:- used to heat solution 2.
A similar. experiment usinga mixture containing 97% sodium. hydroxide and; 3% technicalsodium gluconate gave results similar to those obtained. above with solution2.
A- further advantage obtained in using. a suitable hydroxyv compound as described herein is the. elimination or the substantial reduction of the problems involved. in removing smut often formed during aluminumetching. This smutis ordinarily silicon, carbon, copper on. other materials left at. the surface of the article being etched after. removalv of the aluminum by the etching solution. The. removal of this smut often requires additional treatment in an acid bath. When aluminum and. aluminum base" alloys are treated accordingto the method of this invention the smut that remains can be removed much easier so that the removal time is reduced byv /3 to as compared with similar articles etched in a bath according to the old methods. In many instances, the new method leaves the smut in such a condition that it can be easily rinsed off so that the usual acid treatment is unnecessary.
In testing the methods of this invention it has been observed that crude and technical grades of gluconates and gluconic acid give somewhat better results than the purified material although the reason for this is not understood. The following data illustrates the differences in the crude or technical grade gluconate and the purified material.
In. contrastv to this the materials; used in the present methods produced the. following; comparative results:
-' gpmpafiztivle 11316 0 CB 9 Material Foi-matibnl Hours NaOH only, control 0 Glucoheptonic lactone. +16 Tartaric acid +2 Mucic acid +8 U. S. P. gluconic acid +16 Corn starch +11 Glucolactone +16 Glucose +4 Lactose +4 Glycerine. +1 Sorbitol +16 Gum arabio. +16
A preferred composition for use in applicants? method is made up of 96% by' weight of sodium hydroxide and 1% of technical 50% gluconic acid. This acid, of course, is converted immedi-- ately to sodium gluconate.
In the preferred method, the solution is main-- tained at a temperature of from 120 F. to 210 F during the treatment and the polyhydroxy compound is present in an amount of 0.5% to 10% by weight of the combined alkali and the com-- pound. In the preferred solutions the alkali is: present in an amount of 4.0% to 10.0% by weight of the solution.
Having described our invention as related to the embodiments disclosed herein it is our inten- Solu- 10 oz./ga1.0f mix com- Per- Precipitate Obtion posed of cent Aluminum added served After- 1 NaOH 100 Theoretical amount lhour.
for caustic present. NaOH 95 2 Purified sodium glu- 5 do hours.
conate. NaOH 99.5 3 Purified sodium glu- .5 do l8ho11rs.
conate. NaOH 99.5 4 Crude sodium glu- .5 do 36hours.
conate. NaOH 97 5 Crude sodium glu- 3 do None formed for conate. 170 hours. aOH 97 6 Tech. sodium glu- 3 -.do 96hours.
conate.
Comparative Time of Scale Formation, Hours Material NaOH only, Control Itaconic acid Sorbic acicl Aconitic acid 2,4 dimethylene glucomc acid. Lactic acid Citric acid Tetra sodium salt of ethylene d1amme tetra acetic acid Ethylene glycol tion that the invention be not limited by any of the details of description unless otherwise specified but rather be construed broadly within its spirit and scope as set out in accompanying claims.
We claim:
1. In the etching of articles of aluminum and of aluminum base alloys, the method which comprises treating the surface of said article with a hot aqueous solution comprising an etching alkali and a small amount of water-soluble saturated aliphatic polyhydroxy compound in a proportion such that the formation of a hard adherent precipitate is avoided for an extended period of time, said compound being selected from the class consisting of polyhydric alcohols of the formula CI-IzOI-HCHOHMCHzOH wherein a is at least 2, starches of the formula (C6H10O5)z, polyhydroxy monobasic acids of the formula COOH(CHOH) cCH2OH wherein c is at least 4, polyhydroxy dibasic acids of the formula COOH CHOH COOH wherein (Z is at least 3, gum arabic and the alkali metal salts of said acids.
2. The method of claim 1 wherein said polyhydroxy compound is present in an amount of 0.1% to 20.0% by weight of the combined alkali and said compound.
3. The method of claim 1 wherein said solution is maintained at a temperature of 60 to 212 F. during said treatment.
4. The method of claim 1 wherein said polyhydroxy compound is present in an amount of 0.1% to 20.0% by weight of the combined alkali and said compound, the solution is maintained at a temperature of 60 to 212 F. during said treatment, and the alkali is present in an amount of 2.0% to 20.0% by weight of the solution.
5. The method of claim 4 wherein said alkali comprises sodium hydroxide and said polyhydroxy compound comprises sodium gluconate.
6. In the etching of articles of aluminum and of aluminum base alloys, the method which comprises treating the surface of said article with an aqueous solution containing ounces per gallon of a mixture of 98% by weight of sodium hydroxide and 2% by weight of sodium gluconate while maintaining said solution at a temperature of about to F.
7. The method of claim 1, wherein said aliphatic polyhydroxy compound is glucoheptonic lactone.
8. The method of claim 1, wherein said aliphatic polyhydroxy compound is gluconolactone.
9. The method of claim 1, wherein said aliphatic polyhydroxy compound is gluconic acid.
10. The method of claim 1, wherein said aliphatic polyhydroxy compound is music acid.
11. The method of claim 1, wherein said aliphatic polyhydroxy compound is sorbitol.
VLADIMIR DVORKOVITZ. JOHN R. SWIHART.
References Cited in the file 0! this patent UNITED STATES PATENTS Number
Claims (1)
1. IN THE ETCHING OF ARTICLES OF ALUMINUM AND OF ALUMINUM BASE ALLOYS, THE METHOD WHICH COMPRISES TREATING THE SURFACE OF SAID ARTICLE WITH A HOT AQUEOUS SOLUTION COMPRISING AN ETCHING ALKALI AND A SMALL AMOUNT OF WATER-SOLUBLE SATURATED ALIPHATIC POLYHYDROXY COMPOUND IN A PROPORTION SUCH THAT THE FORMATION OF A HARD ADHERENT PRECIPITATE IS AVOIDED FOR AN EXTENDED PERIOD OF TIME, SAID COMPOUND BEING SELECTED FROM THE CLASS CONSISTING OF POLYHYDRIC ALCHOLS OF THE FORMULA CH2OH(CHOH)CH OH WHERIN A IS AT LEAST 2, STARCHES OF THE FORMULA (C6H10O5)X, POLYHYDROXY MONOBASIC ACIDS OF THE FORMULA
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Cited By (31)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2739883A (en) * | 1954-07-22 | 1956-03-27 | Turco Products Inc | Process of etching aluminum |
US2741051A (en) * | 1954-09-23 | 1956-04-10 | Allied Chem & Dye Corp | Process for controlling scale formation in aluminum etching |
US2756131A (en) * | 1952-08-22 | 1956-07-24 | Vaw Ver Aluminium Werke Ag | Method for glossing articles made of aluminum and particularly pure aluminum and its alloys |
US2795490A (en) * | 1955-01-31 | 1957-06-11 | Turco Products Inc | Process for etching aluminum alloy surfaces |
US2839370A (en) * | 1956-05-04 | 1958-06-17 | Hanson Van Winkle Munning Co | Aluminum etching |
US2853372A (en) * | 1954-11-22 | 1958-09-23 | Kelite Products Inc | Composition and process for the controlled etching of aluminum and aluminum alloys |
US2869267A (en) * | 1957-02-28 | 1959-01-20 | Turco Products Inc | Method of etching aluminum and aluminum alloys |
US2872301A (en) * | 1955-03-31 | 1959-02-03 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US2882134A (en) * | 1954-12-08 | 1959-04-14 | Pennsalt Chemicals Corp | Process for aluminum etching |
US2918357A (en) * | 1955-11-02 | 1959-12-22 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US2931713A (en) * | 1957-09-27 | 1960-04-05 | Amchem Prod | Method of and material for etching aluminum |
US2940877A (en) * | 1955-04-21 | 1960-06-14 | Gen Motors Corp | Paint stripping composition |
US2942955A (en) * | 1957-05-20 | 1960-06-28 | Wyandotte Chemicals Corp | Aluminum etching composition and method |
US2962395A (en) * | 1960-11-29 | Paint stripping method and composition | ||
US2965457A (en) * | 1957-05-01 | 1960-12-20 | Du Pont | Process for etching aluminum |
US2975040A (en) * | 1955-11-02 | 1961-03-14 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US2975041A (en) * | 1956-08-06 | 1961-03-14 | Purex Corp Ltd | Method for etching aluminum and aluminum alloy bodies |
US2975039A (en) * | 1955-11-02 | 1961-03-14 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US2976248A (en) * | 1957-08-01 | 1961-03-21 | Wyandotte Chemicals Corp | Bottle washing composition and method |
US2992187A (en) * | 1958-04-18 | 1961-07-11 | Pfister Chemical Works Inc | Method of removing rust |
US2992998A (en) * | 1956-03-19 | 1961-07-18 | Olin Mathieson | Fructoheptonate inhibited alkaline detergent solutions |
US3085917A (en) * | 1960-05-27 | 1963-04-16 | Gen Electric | Chemical cleaning method and material |
US3095380A (en) * | 1958-07-14 | 1963-06-25 | Purex Corp Ltd | Composition for removal of heat scale and carbon deposits |
US3105822A (en) * | 1956-03-01 | 1963-10-01 | Olin Mathieson | Inhibited alkaline detergent solution |
US3210287A (en) * | 1960-05-06 | 1965-10-05 | Wyandotte Chemicals Corp | Nonstaining aluminum cleaning composition and method |
US3298832A (en) * | 1962-09-26 | 1967-01-17 | Polaroid Corp | Copper gluconate containing receiving element and its diffusion transfer photography use |
US3486954A (en) * | 1966-02-07 | 1969-12-30 | Mc Donnell Douglas Corp | Method for etching aluminum |
US3622470A (en) * | 1969-05-21 | 1971-11-23 | Wire & Strip Platers Inc | Continuous plating method |
US4504324A (en) * | 1983-11-07 | 1985-03-12 | Nippon Paint Co., Ltd. | Surface treatment of aluminum materials |
US5114607A (en) * | 1990-08-08 | 1992-05-19 | Betz Laboratories, Inc. | Low foaming alkaline cleaner comprising a surfactant mixture of an EO-PO-EO block copolymer and a PO-ZO-PO block copolymer |
IT201800010025A1 (en) * | 2018-11-05 | 2020-05-05 | Simet S R L | Process for the surface treatment of metals using a chemical bath. |
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US2318559A (en) * | 1941-04-30 | 1943-05-04 | Monsanto Chemicals | Material for and process of pickling copper or its alloys |
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US2168909A (en) * | 1936-12-01 | 1939-08-08 | Aluminum Co Of America | Producing etched surfaces on aluminum |
US2318559A (en) * | 1941-04-30 | 1943-05-04 | Monsanto Chemicals | Material for and process of pickling copper or its alloys |
Cited By (32)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2962395A (en) * | 1960-11-29 | Paint stripping method and composition | ||
US2756131A (en) * | 1952-08-22 | 1956-07-24 | Vaw Ver Aluminium Werke Ag | Method for glossing articles made of aluminum and particularly pure aluminum and its alloys |
US2739883A (en) * | 1954-07-22 | 1956-03-27 | Turco Products Inc | Process of etching aluminum |
US2741051A (en) * | 1954-09-23 | 1956-04-10 | Allied Chem & Dye Corp | Process for controlling scale formation in aluminum etching |
US2853372A (en) * | 1954-11-22 | 1958-09-23 | Kelite Products Inc | Composition and process for the controlled etching of aluminum and aluminum alloys |
US2882134A (en) * | 1954-12-08 | 1959-04-14 | Pennsalt Chemicals Corp | Process for aluminum etching |
US2795490A (en) * | 1955-01-31 | 1957-06-11 | Turco Products Inc | Process for etching aluminum alloy surfaces |
US2872301A (en) * | 1955-03-31 | 1959-02-03 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US2940877A (en) * | 1955-04-21 | 1960-06-14 | Gen Motors Corp | Paint stripping composition |
US2918357A (en) * | 1955-11-02 | 1959-12-22 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US2975040A (en) * | 1955-11-02 | 1961-03-14 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US2975039A (en) * | 1955-11-02 | 1961-03-14 | Pennsalt Chemicals Corp | Chemical composition and process for aluminum etching |
US3105822A (en) * | 1956-03-01 | 1963-10-01 | Olin Mathieson | Inhibited alkaline detergent solution |
US2992998A (en) * | 1956-03-19 | 1961-07-18 | Olin Mathieson | Fructoheptonate inhibited alkaline detergent solutions |
US2839370A (en) * | 1956-05-04 | 1958-06-17 | Hanson Van Winkle Munning Co | Aluminum etching |
US2975041A (en) * | 1956-08-06 | 1961-03-14 | Purex Corp Ltd | Method for etching aluminum and aluminum alloy bodies |
US2869267A (en) * | 1957-02-28 | 1959-01-20 | Turco Products Inc | Method of etching aluminum and aluminum alloys |
US2965457A (en) * | 1957-05-01 | 1960-12-20 | Du Pont | Process for etching aluminum |
US2942955A (en) * | 1957-05-20 | 1960-06-28 | Wyandotte Chemicals Corp | Aluminum etching composition and method |
US2976248A (en) * | 1957-08-01 | 1961-03-21 | Wyandotte Chemicals Corp | Bottle washing composition and method |
US2931713A (en) * | 1957-09-27 | 1960-04-05 | Amchem Prod | Method of and material for etching aluminum |
US2992187A (en) * | 1958-04-18 | 1961-07-11 | Pfister Chemical Works Inc | Method of removing rust |
US3095380A (en) * | 1958-07-14 | 1963-06-25 | Purex Corp Ltd | Composition for removal of heat scale and carbon deposits |
US3210287A (en) * | 1960-05-06 | 1965-10-05 | Wyandotte Chemicals Corp | Nonstaining aluminum cleaning composition and method |
US3085917A (en) * | 1960-05-27 | 1963-04-16 | Gen Electric | Chemical cleaning method and material |
US3298832A (en) * | 1962-09-26 | 1967-01-17 | Polaroid Corp | Copper gluconate containing receiving element and its diffusion transfer photography use |
US3486954A (en) * | 1966-02-07 | 1969-12-30 | Mc Donnell Douglas Corp | Method for etching aluminum |
US3622470A (en) * | 1969-05-21 | 1971-11-23 | Wire & Strip Platers Inc | Continuous plating method |
US4504324A (en) * | 1983-11-07 | 1985-03-12 | Nippon Paint Co., Ltd. | Surface treatment of aluminum materials |
US5114607A (en) * | 1990-08-08 | 1992-05-19 | Betz Laboratories, Inc. | Low foaming alkaline cleaner comprising a surfactant mixture of an EO-PO-EO block copolymer and a PO-ZO-PO block copolymer |
IT201800010025A1 (en) * | 2018-11-05 | 2020-05-05 | Simet S R L | Process for the surface treatment of metals using a chemical bath. |
US11220752B2 (en) | 2018-11-05 | 2022-01-11 | Simet S.R.L. | Process for surface treatment of aluminum or aluminum alloys by an alkaline chemical bath |
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