JP2024037088A - Method for forming lubricating layer on surface of metal material and method for manufacturing lubricating layer-containing metal material - Google Patents
Method for forming lubricating layer on surface of metal material and method for manufacturing lubricating layer-containing metal material Download PDFInfo
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- 239000007769 metal material Substances 0.000 title claims abstract description 111
- 238000000034 method Methods 0.000 title claims abstract description 80
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 68
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 81
- 239000000344 soap Substances 0.000 claims abstract description 42
- 229910052751 metal Inorganic materials 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims abstract description 38
- 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 claims abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 21
- 239000011734 sodium Substances 0.000 claims abstract description 21
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 20
- 239000011591 potassium Substances 0.000 claims abstract description 20
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 12
- 239000011701 zinc Substances 0.000 claims abstract description 12
- 239000000314 lubricant Substances 0.000 claims description 56
- 229910052782 aluminium Inorganic materials 0.000 claims description 36
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 35
- 229910052749 magnesium Inorganic materials 0.000 claims description 31
- 239000011777 magnesium Substances 0.000 claims description 31
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 19
- -1 magnesium halides Chemical class 0.000 claims description 16
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 11
- 229930195729 fatty acid Natural products 0.000 claims description 11
- 239000000194 fatty acid Substances 0.000 claims description 11
- 150000004665 fatty acids Chemical class 0.000 claims description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 8
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 6
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 4
- 239000003513 alkali Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000007781 pre-processing Methods 0.000 abstract 2
- 239000000463 material Substances 0.000 description 31
- 229940091250 magnesium supplement Drugs 0.000 description 29
- 239000007864 aqueous solution Substances 0.000 description 25
- 239000004927 clay Substances 0.000 description 23
- 239000004033 plastic Substances 0.000 description 20
- 238000005461 lubrication Methods 0.000 description 11
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 8
- MBMBGCFOFBJSGT-KUBAVDMBSA-N all-cis-docosa-4,7,10,13,16,19-hexaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCC(O)=O MBMBGCFOFBJSGT-KUBAVDMBSA-N 0.000 description 8
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 8
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 8
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 8
- ZQPPMHVWECSIRJ-MDZDMXLPSA-N elaidic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(O)=O ZQPPMHVWECSIRJ-MDZDMXLPSA-N 0.000 description 8
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 8
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 8
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 8
- SECPZKHBENQXJG-FPLPWBNLSA-N palmitoleic acid Chemical compound CCCCCC\C=C/CCCCCCCC(O)=O SECPZKHBENQXJG-FPLPWBNLSA-N 0.000 description 8
- CIOMGYGRGMIGFM-UHFFFAOYSA-I [F-].[F-].[F-].[F-].[F-].[Al+3].[Zn++] Chemical compound [F-].[F-].[F-].[F-].[F-].[Al+3].[Zn++] CIOMGYGRGMIGFM-UHFFFAOYSA-I 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000012669 compression test Methods 0.000 description 5
- 229960002337 magnesium chloride Drugs 0.000 description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 description 5
- 235000011147 magnesium chloride Nutrition 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 4
- 235000021357 Behenic acid Nutrition 0.000 description 4
- 239000005639 Lauric acid Substances 0.000 description 4
- 235000021353 Lignoceric acid Nutrition 0.000 description 4
- CQXMAMUUWHYSIY-UHFFFAOYSA-N Lignoceric acid Natural products CCCCCCCCCCCCCCCCCCCCCCCC(=O)OCCC1=CC=C(O)C=C1 CQXMAMUUWHYSIY-UHFFFAOYSA-N 0.000 description 4
- 239000005642 Oleic acid Substances 0.000 description 4
- 235000021314 Palmitic acid Nutrition 0.000 description 4
- 235000021319 Palmitoleic acid Nutrition 0.000 description 4
- 235000021355 Stearic acid Nutrition 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 4
- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 4
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 4
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 4
- 229940114079 arachidonic acid Drugs 0.000 description 4
- 235000021342 arachidonic acid Nutrition 0.000 description 4
- 229940116226 behenic acid Drugs 0.000 description 4
- SECPZKHBENQXJG-UHFFFAOYSA-N cis-palmitoleic acid Natural products CCCCCCC=CCCCCCCCC(O)=O SECPZKHBENQXJG-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 235000020669 docosahexaenoic acid Nutrition 0.000 description 4
- 229940090949 docosahexaenoic acid Drugs 0.000 description 4
- 235000020673 eicosapentaenoic acid Nutrition 0.000 description 4
- 229960005135 eicosapentaenoic acid Drugs 0.000 description 4
- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 4
- FARYTWBWLZAXNK-WAYWQWQTSA-N ethyl (z)-3-(methylamino)but-2-enoate Chemical compound CCOC(=O)\C=C(\C)NC FARYTWBWLZAXNK-WAYWQWQTSA-N 0.000 description 4
- 238000009778 extrusion testing Methods 0.000 description 4
- 229960004488 linolenic acid Drugs 0.000 description 4
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 4
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000002203 pretreatment Methods 0.000 description 4
- 235000003441 saturated fatty acids Nutrition 0.000 description 4
- 150000004671 saturated fatty acids Chemical class 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 4
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 4
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 238000005242 forging Methods 0.000 description 3
- 238000005555 metalworking Methods 0.000 description 3
- 235000021313 oleic acid Nutrition 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 238000005491 wire drawing Methods 0.000 description 3
- 150000003752 zinc compounds Chemical class 0.000 description 3
- BHHYHSUAOQUXJK-UHFFFAOYSA-L zinc fluoride Chemical compound F[Zn]F BHHYHSUAOQUXJK-UHFFFAOYSA-L 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013527 degreasing agent Substances 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- BLQJIBCZHWBKSL-UHFFFAOYSA-L magnesium iodide Chemical compound [Mg+2].[I-].[I-] BLQJIBCZHWBKSL-UHFFFAOYSA-L 0.000 description 2
- 229910001641 magnesium iodide Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 2
- 229940007718 zinc hydroxide Drugs 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000617482 Kiwa Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Extrusion Of Metal (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
Description
本発明は、金属材料表面への潤滑層形成方法、及び潤滑層含有金属材料の製造方法に関する。 The present invention relates to a method for forming a lubricant layer on the surface of a metal material, and a method for producing a metal material containing a lubricant layer.
金属材料の鍛造、伸線、伸管、ロールフォーミング、プレスなどの塑性加工において発生する摩擦は、加工エネルギーの増大、発熱などの原因となる。このため、従来、塑性加工には、種々の潤滑剤が用いられている。潤滑剤としては、例えば、鉱油、合成油、植物油などの液体状の潤滑剤が古くから用いられている。しかしながら、これらの潤滑剤は、比較的簡易な塑性加工には適用し得るものの、高い面圧下で摺動して大きな発熱を伴う塑性加工においては、潤滑性能が不十分である。 Friction that occurs during plastic processing such as forging, wire drawing, pipe drawing, roll forming, and pressing of metal materials causes an increase in processing energy and heat generation. For this reason, various lubricants have conventionally been used in plastic working. As the lubricant, for example, liquid lubricants such as mineral oil, synthetic oil, and vegetable oil have been used for a long time. However, although these lubricants can be applied to relatively simple plastic working, their lubrication performance is insufficient in plastic working that involves sliding under high surface pressure and generates large amounts of heat.
そこで、大きな発熱を伴うような塑性加工においては、金属材料表面に固体皮膜を形成して、金型などの加工具と加工対象である金属材料とが直接接触することを抑制する方法が広く採用されている。 Therefore, in plastic processing that generates a large amount of heat, a method is widely adopted in which a solid film is formed on the surface of the metal material to prevent direct contact between processing tools such as molds and the metal material being processed. has been done.
固体皮膜を形成して金属材料の加工性を高める方法としては、例えば、加工時の材料流動化と材料表面の焼き付きを防止するために、例えばアルミニウムの場合は、材料表面に潤滑皮膜化成処理（フッ化アルミニウム亜鉛処理）を行う方法が広く採用されている。具体的には、フッ化亜鉛（ＺｎＦ2）とケイフッ化ソーダの水溶液を用いて、アルミニウム表面にフッ化アルミニウムとフッ化亜鉛の皮膜を形成させ、この亜鉛化合物と潤滑剤である石けんとの皮膜（金属石けん）を作ることで、表面潤滑性を担保している。 As a method to improve the workability of metal materials by forming a solid film, for example, in the case of aluminum, in order to prevent material fluidization during processing and seizure of the material surface, a lubricating film chemical conversion treatment ( Aluminum fluoride zinc treatment) is widely used. Specifically, an aqueous solution of zinc fluoride (ZnF 2 ) and sodium silicofluoride is used to form a film of aluminum fluoride and zinc fluoride on the aluminum surface, and a film of this zinc compound and soap, which is a lubricant, is formed on the aluminum surface. (metallic soap) ensures surface lubricity.
しかしながら、皮膜処理液には、反応に伴いアルミニウムイオンが堆積して反応を阻害するようになるため、頻繁な処理液の更新が不可欠である。 However, as aluminum ions accumulate in the coating treatment solution as the reaction progresses and inhibit the reaction, frequent renewal of the treatment solution is essential.
例えば、特許文献１は、亜鉛化合物の水溶液を用いて、アルミニウム表面に粘土化膜（層状複水酸化物）を形成する手法を開示している。この粘土化膜は、亜鉛水酸化物とアルミニウム水酸化物を主成分とする層構造をした粘土物質であり、アルミニウムを亜鉛水溶液に浸漬するだけの簡易プロセスにより形成される。 For example, Patent Document 1 discloses a method of forming a clay film (layered double hydroxide) on an aluminum surface using an aqueous solution of a zinc compound. This clay film is a clay material with a layered structure mainly composed of zinc hydroxide and aluminum hydroxide, and is formed by a simple process of immersing aluminum in an aqueous zinc solution.
このため、特許文献１に開示された粘土化膜を合成する手法（粘土化法）は、既存方法であるフッ化アルミ亜鉛処理と置き換え可能といえる。また、粘土化膜には、潤滑剤である石けんと結びつきの強い亜鉛水酸化物が含まれていることから、アルミニウム表面に潤滑皮膜を形成することができる。また、この粘土化法は、フッ化アルミニウム亜鉛処理法のように、皮膜処理液中にアルミニウムが堆積することがないため、処理液の頻繁な更新は必要としないという利点も有している。さらには、前述のフッ化アルミニウム亜鉛処理のように有害物質であるフッ素を使用する必要が無いという利点も有している。 Therefore, it can be said that the method of synthesizing a clay film disclosed in Patent Document 1 (clay formation method) can be replaced with the existing method of aluminum zinc fluoride treatment. In addition, since the argillaceous film contains zinc hydroxide, which has a strong bond with soap, which is a lubricant, a lubricating film can be formed on the aluminum surface. Furthermore, unlike the aluminum zinc fluoride treatment method, this clay forming method does not deposit aluminum in the film treatment solution, and therefore has the advantage that frequent renewal of the treatment solution is not required. Furthermore, it has the advantage that there is no need to use fluorine, which is a harmful substance, unlike the above-mentioned aluminum zinc fluoride treatment.
しかしながら、特許文献１の粘土化法の反応時間は、２４時間以上を必要とするため、実用化には課題が残っている。また、特許文献１の粘土化法によって形成された粘土化膜と、潤滑剤（石けん）とは、複合膜を形成するが、当該複合膜の潤滑性をさらに高めることも求められる。 However, since the reaction time of the clay forming method of Patent Document 1 requires 24 hours or more, problems remain in practical application. Further, the clay film formed by the clay formation method of Patent Document 1 and the lubricant (soap) form a composite film, but it is also required to further improve the lubricity of the composite film.
このような状況下、本出願人は、カルシウム、カリウム及びナトリウムの少なくとも１種類を含むアルカリ成分を含有する水性液体である金属表面前処理剤を、金属材料表面に接触させ、その後、前記金属表面前処理剤が付着した金属材料表面に、亜鉛化合物を含む皮膜形成用処理剤を接触させて金属材料表面に亜鉛を含む皮膜を形成する、皮膜形成処理方法を提供した（特許文献２参照）。 Under these circumstances, the present applicant brought a metal surface pretreatment agent, which is an aqueous liquid containing an alkaline component containing at least one of calcium, potassium, and sodium, into contact with the surface of the metal material, and then A film-forming treatment method was provided in which a film-forming treatment agent containing a zinc compound is brought into contact with the surface of a metal material to which a pre-treatment agent has been adhered to form a film containing zinc on the surface of the metal material (see Patent Document 2).
特許文献２に記載の当該方法は、金属材料表面に亜鉛を含む皮膜を迅速に形成できる利点がある。そして、当該皮膜に潤滑剤を適用することにより、金属材料の塑性加工において優れた潤滑性が発揮されることが記載されている。 The method described in Patent Document 2 has the advantage that a film containing zinc can be quickly formed on the surface of a metal material. It is also described that by applying a lubricant to the film, excellent lubricity can be exhibited in plastic working of metal materials.
しかし、特許文献２に記載の皮膜形成処理方法は、重金属である亜鉛を使用しており、環境負荷の面で改善の余地があった。 However, the film forming treatment method described in Patent Document 2 uses zinc, which is a heavy metal, and there is room for improvement in terms of environmental impact.
本発明は、上記課題を解決するものであり、亜鉛を使用しないため環境負荷が小さい、金属材料表面への潤滑層形成方法、及び潤滑層含有金属材料の製造方法を提供することを目的とする。 The present invention solves the above problems, and aims to provide a method for forming a lubricant layer on the surface of a metal material and a method for manufacturing a metal material containing a lubricant layer, which has a small environmental impact because zinc is not used. .
本発明者は、上記のような課題を解決すべく鋭意検討を行った。その結果、カリウム及びナトリウムの少なくとも１種を含むアルカリ成分を含有する金属表面前処理剤を金属材料表面に接触させて前処理し、その後、マグネシウム化合物を含有する皮膜形成用処理剤を前処理した金属材料表面に接触させて皮膜を形成し、さらに、石鹸を含有する潤滑層形成用処理剤を前記皮膜に接触させることにより、金属材料表面に優れた潤滑性を発揮する潤滑層を形成できることを見出した。本発明は、これらの知見に基づいて、さらに検討を重ねることにより完成された発明である。 The present inventor conducted extensive studies to solve the above problems. As a result, a metal surface pretreatment agent containing an alkaline component containing at least one of potassium and sodium was brought into contact with the surface of the metal material for pretreatment, and then a film-forming treatment agent containing a magnesium compound was pretreated. It has been shown that a lubricant layer exhibiting excellent lubricity can be formed on the surface of a metal material by contacting the surface of the metal material to form a film, and further contacting the film with a treatment agent for forming a lubricant layer containing soap. I found it. The present invention was completed through further studies based on these findings.
すなわち、本発明は、下記に掲げる態様の発明を提供する。
項１． カリウム及びナトリウムの少なくとも１種を含むアルカリ成分を含有する金属表面前処理剤を金属材料表面に接触させて前処理する前処理工程、マグネシウム化合物を含有する皮膜形成用処理剤を前処理した金属材料表面に接触させて皮膜を形成する皮膜形成工程、及び石鹸を含有する潤滑層形成用処理剤を前記皮膜に接触させて潤滑層を形成する潤滑層形成工程を含む、金属材料表面への潤滑層形成方法。
項２． 前記アルカリ成分が、水酸化カリウム及び水酸化ナトリウムの少なくとも１種を含む、項１に記載の金属材料表面への潤滑層形成方法。
項３． 前記金属表面前処理剤中の前記アルカリ成分の濃度が、０．０１～１０ｍｏｌ／Ｌである、項１又は２に記載の金属材料表面への潤滑層形成方法。
項４． 前記金属材料表面が、アルミニウム、亜鉛、マグネシウム、鉄、銅、またはこれらの金属のうち少なくとも１種を含む合金により構成されている、項１～３のいずれか１項に記載の金属材料表面への潤滑層形成方法。
項５． 前記マグネシウム化合物が、ハロゲン化マグネシウム、硝酸マグネシウム、及び硫酸マグネシウムからなる群より選択される１種以上である、項１～４のいずれか１項に記載の金属材料表面への潤滑層形成方法。
項６． 前記皮膜形成用処理剤中の前記マグネシウム化合物の濃度が、０．０１～１０ｍｏｌ／Ｌである、項１～５のいずれか１項に記載の金属材料表面への潤滑層形成方法。
項７． 前記石鹸が、炭素数１２～２０の脂肪酸のアルカリ金属塩である、項１～６のいずれか１項に記載の金属材料表面への潤滑層形成方法。
項８． 前記潤滑層形成用処理剤中の前記石鹸の濃度が、０．０１～１０ｍｏｌ／Ｌである、項１～７のいずれか１項に記載の金属材料表面への潤滑層形成方法。
項９． カリウム及びナトリウムの少なくとも１種を含むアルカリ成分を含有する金属表面前処理剤を金属材料表面に接触させて前処理する前処理工程、マグネシウム化合物を含有する皮膜形成用処理剤を前処理した金属材料表面に接触させて皮膜を形成する皮膜形成工程、及び石鹸を含有する潤滑層形成用処理剤を前記皮膜に接触させて潤滑層を形成する潤滑層形成工程を含む、潤滑層含有金属材料の製造方法。
That is, the present invention provides inventions of the following aspects.
Item 1. A pretreatment step of pretreating the surface of a metal material by contacting it with a metal surface pretreatment agent containing an alkaline component containing at least one of potassium and sodium, and a metal material pretreated with a film-forming treatment agent containing a magnesium compound. A lubricating layer on the surface of a metal material, including a film forming step of contacting the surface to form a film, and a lubricating layer forming step of bringing a soap-containing lubricating layer forming treatment agent into contact with the film to form a lubricating layer. Formation method.
Item 2. Item 2. The method for forming a lubricating layer on the surface of a metal material according to Item 1, wherein the alkaline component contains at least one of potassium hydroxide and sodium hydroxide.
Item 3. Item 3. The method for forming a lubricating layer on the surface of a metal material according to Item 1 or 2, wherein the concentration of the alkaline component in the metal surface pretreatment agent is 0.01 to 10 mol/L.
Item 4. To the metal material surface according to any one of Items 1 to 3, wherein the metal material surface is made of aluminum, zinc, magnesium, iron, copper, or an alloy containing at least one of these metals. A method for forming a lubricating layer.
Item 5. Item 5. The method for forming a lubricating layer on the surface of a metal material according to any one of Items 1 to 4, wherein the magnesium compound is one or more selected from the group consisting of magnesium halides, magnesium nitrate, and magnesium sulfate.
Item 6. Item 6. The method for forming a lubricating layer on the surface of a metal material according to any one of Items 1 to 5, wherein the concentration of the magnesium compound in the film forming treatment agent is 0.01 to 10 mol/L.
Section 7. Item 7. The method for forming a lubricating layer on the surface of a metal material according to any one of Items 1 to 6, wherein the soap is an alkali metal salt of a fatty acid having 12 to 20 carbon atoms.
Section 8. Item 8. The method for forming a lubricant layer on the surface of a metal material according to any one of Items 1 to 7, wherein the concentration of the soap in the treatment agent for forming a lubricant layer is 0.01 to 10 mol/L.
Item 9. A pretreatment step of pretreating the surface of a metal material by contacting it with a metal surface pretreatment agent containing an alkaline component containing at least one of potassium and sodium, and a metal material pretreated with a film-forming treatment agent containing a magnesium compound. Production of a lubricating layer-containing metal material, including a film forming step of contacting the surface to form a film, and a lubricating layer forming step of bringing a soap-containing lubricating layer forming treatment agent into contact with the film to form a lubricating layer. Method.
本発明の潤滑層形成方法は、有害物質であるフッ素、及び重金属である亜鉛を使用しないため環境負荷が小さく、しかも金属材料表面に、簡易かつ製造効率よく潤滑性に優れる潤滑層を形成することができるという利点がある。また、本発明の潤滑層形成方法によって得られる潤滑層は、金属材料表面に強固に付着しているため剥離しにくいものである。そのため、本発明の潤滑層形成方法は、金属材料を塑性加工する金属加工工程を含む金属加工方法に好適に適用することができる。 The method for forming a lubricant layer of the present invention has a small environmental impact because it does not use fluorine, which is a harmful substance, or zinc, which is a heavy metal.Moreover, it forms a lubricant layer with excellent lubricity on the surface of a metal material easily and efficiently. It has the advantage of being able to Further, the lubricant layer obtained by the lubricant layer forming method of the present invention is firmly attached to the surface of the metal material and is therefore difficult to peel off. Therefore, the lubricating layer forming method of the present invention can be suitably applied to a metal working method including a metal working step of plastic working a metal material.
＜金属材料表面への潤滑層形成方法＞
本発明の金属材料表面への潤滑層形成方法は、カリウム及びナトリウムの少なくとも１種を含むアルカリ成分を含有する金属表面前処理剤を金属材料表面に接触させて前処理する前処理工程、マグネシウム化合物を含有する皮膜形成用処理剤を前処理した金属材料表面に接触させて皮膜を形成する皮膜形成工程、及び石鹸を含有する潤滑層形成用処理剤を前記皮膜に接触させて潤滑層を形成する潤滑層形成工程を含む。
<Method for forming a lubricant layer on the surface of metal materials>
The method for forming a lubricating layer on the surface of a metal material according to the present invention includes a pretreatment step in which a metal surface pretreatment agent containing an alkaline component containing at least one of potassium and sodium is brought into contact with the surface of the metal material. A film forming step in which a film-forming treatment agent containing soap is brought into contact with the surface of a pretreated metal material to form a film, and a lubricant layer-forming treatment agent containing soap is brought into contact with the film to form a lubricant layer. Includes a lubricant layer forming step.
前記金属表面前処理剤を金属材料表面に接触（付着）させて前処理することにより、金属材料表面にカリウム及び／又はナトリウムを含む粘土化膜が形成される。当該粘土化膜にマグネシウム化合物を含有する皮膜形成用処理剤を接触（付着）させることにより、当該粘土化膜中のカリウム及び／又はナトリウムがマグネシウムにイオン置換され、マグネシウムを含む皮膜（粘土化膜）が形成される。そして、マグネシウムを含む皮膜に石鹸を含有する潤滑層形成用処理剤を接触（付着）させることにより、石鹸中のアルカリ金属がマグネシウムにイオン置換され、マグネシウム金属石鹸を含む潤滑層が形成される。当該潤滑層は、金属材料表面に強固に付着しているため剥離しにくく、金属材料の塑性加工において優れた潤滑性を発揮する。そのため、当該潤滑層を有する金属材料は、優れた塑性加工性を有する。以下、本発明の金属材料表面への潤滑層形成方法における各工程について詳述する。 A clay film containing potassium and/or sodium is formed on the surface of the metal material by contacting (adhering) the metal surface pretreatment agent to the surface of the metal material for pretreatment. By contacting (adhering) a film-forming treatment agent containing a magnesium compound to the clay film, potassium and/or sodium in the clay film is ion-replaced with magnesium, forming a magnesium-containing film (clay film). ) is formed. Then, by contacting (adhering) a treatment agent for forming a lubricating layer containing soap to the film containing magnesium, the alkali metal in the soap is ion-replaced with magnesium, and a lubricating layer containing magnesium metal soap is formed. The lubricating layer is firmly attached to the surface of the metal material, so it is difficult to peel off, and exhibits excellent lubricity during plastic working of the metal material. Therefore, the metal material having the lubricating layer has excellent plastic workability. Each step in the method for forming a lubricant layer on the surface of a metal material according to the present invention will be described in detail below.
〔前処理工程〕
前処理工程は、カリウム及びナトリウムの少なくとも１種を含むアルカリ成分を含有する金属表面前処理剤を金属材料表面に接触（付着）させて前処理する工程である。当該前処理により、金属材料表面にカリウム及び／又はナトリウムを含む粘土化膜が形成される。
[Pre-treatment process]
The pretreatment step is a step in which a metal surface pretreatment agent containing an alkali component containing at least one of potassium and sodium is brought into contact with (adhered to) the surface of the metal material to perform pretreatment. Through the pretreatment, a clay film containing potassium and/or sodium is formed on the surface of the metal material.
本発明において、アルカリ成分とは、カリウム及びナトリウムの少なくとも１種を含み、水に溶解すると水酸化物イオンを生じる物質をいう。前記アルカリ成分としては、例えば、アルカリ金属の水酸化物が挙げられるが、好ましくは水酸化カリウム（ＫＯＨ）及び水酸化ナトリウム（ＮａＯＨ）である。また、金属表面前処理剤は、例えば、水溶液である。すなわち、金属表面前処理剤は、好ましくは水酸化カリウムを含む水溶液、水酸化ナトリウムを含む水溶液、又は水酸化カリウムと水酸化ナトリウムを含む水溶液であり、より好ましくは水酸化カリウムを含む水溶液、又は水酸化ナトリウムを含む水溶液である。 In the present invention, the alkaline component refers to a substance that contains at least one of potassium and sodium and generates hydroxide ions when dissolved in water. Examples of the alkali component include alkali metal hydroxides, preferably potassium hydroxide (KOH) and sodium hydroxide (NaOH). Further, the metal surface pretreatment agent is, for example, an aqueous solution. That is, the metal surface pretreatment agent is preferably an aqueous solution containing potassium hydroxide, an aqueous solution containing sodium hydroxide, or an aqueous solution containing potassium hydroxide and sodium hydroxide, more preferably an aqueous solution containing potassium hydroxide, or It is an aqueous solution containing sodium hydroxide.
金属表面前処理剤中のアルカリ成分の濃度（２種以上のアルカリ成分を含む場合は合計濃度）は特に制限されないが、金属材料表面にカリウム及び／又はナトリウムを含む粘土化膜を十分に形成させる観点から、好ましくは０．０１～１０ｍｏｌ／Ｌ、より好ましくは０．０３～５ｍｏｌ／Ｌ、さらに好ましくは０．０５～１ｍｏｌ／Ｌ、特に好ましくは０．０５～０．５ｍｏｌ／Ｌである。 The concentration of the alkaline component in the metal surface pretreatment agent (total concentration if two or more types of alkaline components are included) is not particularly limited, but it is necessary to sufficiently form a clay film containing potassium and/or sodium on the surface of the metal material. From this point of view, it is preferably 0.01 to 10 mol/L, more preferably 0.03 to 5 mol/L, even more preferably 0.05 to 1 mol/L, particularly preferably 0.05 to 0.5 mol/L.
金属表面前処理剤を金属材料表面に接触（付着）させて前処理する際の温度は特に制限されないが、金属材料表面にカリウム及び／又はナトリウムを含む粘土化膜を形成しやすくする観点から、好ましくは２０～９０℃、より好ましくは３０～８０℃、さらに好ましくは４０～７０℃、特に好ましくは４０～６０℃である。 The temperature at which the metal surface pretreatment agent is brought into contact with (adhered to) the surface of the metal material for pretreatment is not particularly limited, but from the viewpoint of facilitating the formation of a clay film containing potassium and/or sodium on the surface of the metal material, The temperature is preferably 20 to 90°C, more preferably 30 to 80°C, even more preferably 40 to 70°C, particularly preferably 40 to 60°C.
金属表面前処理剤を金属材料表面に接触（付着）させる時間は特に制限されないが、金属材料表面にカリウム及び／又はナトリウムを含む粘土化膜を十分に形成させる観点、及び製造効率の観点から、好ましくは３０秒間以上１時間以下、より好ましくは１分間以上３０分間以下、さらに好ましくは２分間以上２０分間以下、特に好ましくは３分間以上１０分間以下である。 The time for contacting (adhering) the metal surface pretreatment agent to the surface of the metal material is not particularly limited, but from the viewpoint of sufficiently forming a clayey film containing potassium and/or sodium on the surface of the metal material, and from the viewpoint of manufacturing efficiency, The duration is preferably 30 seconds or more and 1 hour or less, more preferably 1 minute or more and 30 minutes or less, even more preferably 2 minutes or more and 20 minutes or less, and particularly preferably 3 minutes or more and 10 minutes or less.
金属表面前処理剤を金属材料表面に接触（付着）させる方法は特に制限されず、例えば、ロールコート法、スピンコート法、スプレー法、及び浸漬法などの公知の方法により行うことができる。 The method of bringing the metal surface pretreatment agent into contact with (adhering to) the surface of the metal material is not particularly limited, and can be carried out by known methods such as a roll coating method, a spin coating method, a spray method, and a dipping method.
金属材料を構成する金属は特に制限されないが、好ましくは、アルミニウム、亜鉛、マグネシウム、鉄、銅、またはこれらの金属のうち少なくとも１種を含む合金であり、より好ましくはアルミニウムである。すなわち、金属材料表面は、アルミニウム、亜鉛、マグネシウム、鉄、銅、またはこれらの金属のうち少なくとも１種を含む合金により構成されていることが好ましく、アルミニウムにより構成されていることがより好ましい。 The metal constituting the metal material is not particularly limited, but is preferably aluminum, zinc, magnesium, iron, copper, or an alloy containing at least one of these metals, and more preferably aluminum. That is, the surface of the metal material is preferably made of aluminum, zinc, magnesium, iron, copper, or an alloy containing at least one of these metals, and more preferably made of aluminum.
なお、金属表面前処理剤を金属材料表面に接触（付着）させる前に、金属材料表面を洗浄しておくことが好ましい。金属材料表面の洗浄は、金属材料表面に付着した各種の汚れ（油など）を除去することを主な目的とする。金属材料表面の洗浄方法は特に制限されないが、例えば、アルカリ脱脂剤、及び酸性脱脂剤などの公知の洗浄剤を用いる方法を採用することができる。また、洗浄においては、水洗を行うことが好ましい。 Note that it is preferable to clean the surface of the metal material before contacting (adhering) the metal surface pretreatment agent to the surface of the metal material. The main purpose of cleaning the surface of a metal material is to remove various types of dirt (oil, etc.) attached to the surface of the metal material. The method of cleaning the surface of the metal material is not particularly limited, but for example, a method using a known cleaning agent such as an alkaline degreaser and an acidic degreaser can be adopted. Moreover, in washing, it is preferable to wash with water.
〔皮膜形成工程〕
皮膜形成工程は、マグネシウム化合物を含有する皮膜形成用処理剤を前処理した金属材料表面に接触（付着）させて皮膜を形成する工程である。前処理した金属材料表面にマグネシウム化合物を含有する皮膜形成用処理剤を接触（付着）させることにより、金属材料表面の粘土化膜中のカリウム及び／又はナトリウムがマグネシウムにイオン置換され、マグネシウムを含む皮膜（粘土化膜）が形成される。
[Film formation process]
The film forming step is a step in which a film forming treatment agent containing a magnesium compound is brought into contact with (adhered to) the surface of a pretreated metal material to form a film. By contacting (adhering) a film-forming treatment agent containing a magnesium compound to the surface of the pretreated metal material, the potassium and/or sodium in the clay film on the surface of the metal material is ion-replaced with magnesium, and the magnesium-containing film is ion-replaced with magnesium. A film (clay film) is formed.
マグネシウム化合物は特に制限されないが、ハロゲン化マグネシウム、硝酸マグネシウム、及び硫酸マグネシウムからなる群より選択される１種以上であることが好ましく、より好ましくはハロゲン化マグネシウムであり、さらに好ましくは塩化マグネシウム、臭化マグネシウム、及びヨウ化マグネシウムからなる群より選択される１種以上であり、特に好ましくは塩化マグネシウムである。また、皮膜形成用処理剤は、例えば、水溶液である。すなわち、皮膜形成用処理剤は、好ましくはハロゲン化マグネシウム、硝酸マグネシウム、及び硫酸マグネシウムからなる群より選択される１種以上を含む水溶液であり、より好ましくはハロゲン化マグネシウムを含む水溶液であり、さらに好ましくは塩化マグネシウム、臭化マグネシウム、及びヨウ化マグネシウムからなる群より選択される１種以上を含む水溶液であり、特に好ましくは塩化マグネシウムを含む水溶液である。 The magnesium compound is not particularly limited, but is preferably one or more selected from the group consisting of magnesium halides, magnesium nitrate, and magnesium sulfate, more preferably magnesium halides, and even more preferably magnesium chloride, magnesium sulfate, and magnesium sulfate. One or more types selected from the group consisting of magnesium chloride and magnesium iodide, and particularly preferably magnesium chloride. Further, the film-forming treatment agent is, for example, an aqueous solution. That is, the film-forming treatment agent is preferably an aqueous solution containing one or more selected from the group consisting of magnesium halide, magnesium nitrate, and magnesium sulfate, more preferably an aqueous solution containing magnesium halide, and Preferably, it is an aqueous solution containing one or more selected from the group consisting of magnesium chloride, magnesium bromide, and magnesium iodide, and particularly preferably an aqueous solution containing magnesium chloride.
金属材料表面に形成される、マグネシウムを含む皮膜は、フッ素原子を含まないことが好ましい。すなわち、皮膜形成用処理剤は、フッ素原子を含む成分を含まないことが好ましい。 It is preferable that the film containing magnesium formed on the surface of the metal material does not contain fluorine atoms. That is, it is preferable that the film-forming treatment agent does not contain a component containing a fluorine atom.
皮膜形成用処理剤中のマグネシウム化合物の濃度（２種以上のマグネシウム化合物を含む場合は合計濃度）は特に制限されないが、マグネシウムを含む皮膜を十分に形成させる観点から、好ましくは０．０１～１０ｍｏｌ／Ｌ、より好ましくは０．０５～５ｍｏｌ／Ｌ、さらに好ましくは０．１～１ｍｏｌ／Ｌ、特に好ましくは０．１～０．５ｍｏｌ／Ｌである。 The concentration of the magnesium compound in the film-forming treatment agent (total concentration when two or more types of magnesium compounds are included) is not particularly limited, but from the viewpoint of sufficiently forming a film containing magnesium, it is preferably 0.01 to 10 mol. /L, more preferably 0.05 to 5 mol/L, even more preferably 0.1 to 1 mol/L, particularly preferably 0.1 to 0.5 mol/L.
皮膜形成用処理剤のｐＨは特に制限されないが、前処理した金属材料表面と接触（付着）させることで、マグネシウムを含む皮膜を迅速に形成させる観点から、好ましくは８～１２、より好ましくは９～１１、さらに好ましくは９．５～１０．５である。ｐＨを前記範囲のアルカリ性とする方法としては、例えば、皮膜形成用処理剤にアンモニア水などを添加する方法が挙げられる。 The pH of the film-forming treatment agent is not particularly limited, but is preferably 8 to 12, more preferably 9, from the viewpoint of rapidly forming a film containing magnesium by contacting (adhering) to the surface of the pretreated metal material. -11, more preferably 9.5-10.5. An example of a method for making the pH alkaline within the above range is a method of adding aqueous ammonia or the like to the film-forming treatment agent.
皮膜形成用処理剤を前処理した金属材料表面に接触（付着）させて皮膜を形成する際の温度は特に制限されないが、マグネシウムを含む皮膜を迅速に形成させる観点から、好ましくは５０～９５℃、より好ましくは６０～９０℃、さらに好ましくは７０～８５℃、特に好ましくは７５～８５℃である。 The temperature at which a film is formed by contacting (adhering) the film-forming treatment agent to the surface of a pretreated metal material is not particularly limited, but from the viewpoint of rapidly forming a film containing magnesium, it is preferably 50 to 95°C. , more preferably 60 to 90°C, still more preferably 70 to 85°C, particularly preferably 75 to 85°C.
皮膜形成用処理剤を前処理した金属材料表面に接触（付着）させる時間は特に制限されないが、マグネシウムを含む皮膜を十分に形成させる観点、及び製造効率の観点から、好ましくは３０秒間以上１時間以下、より好ましくは１分間以上３０分間以下、さらに好ましくは２分間以上２０分間以下、特に好ましくは３分間以上１０分間以下である。 The time during which the film-forming treatment agent is brought into contact with (adhered to) the pretreated metal material surface is not particularly limited, but from the viewpoint of sufficiently forming a film containing magnesium and from the viewpoint of manufacturing efficiency, it is preferably 30 seconds or more and 1 hour. Hereinafter, the time period is more preferably 1 minute or more and 30 minutes or less, still more preferably 2 minutes or more and 20 minutes or less, particularly preferably 3 minutes or more and 10 minutes or less.
皮膜形成用処理剤を前処理した金属材料表面に接触（付着）させる方法は特に制限されず、例えば、ロールコート法、スピンコート法、スプレー法、及び浸漬法などの公知の方法により行うことができる。 The method of contacting (adhering) the film-forming treatment agent to the surface of the pretreated metal material is not particularly limited, and for example, known methods such as roll coating, spin coating, spraying, and dipping may be used. can.
〔潤滑層形成工程〕
潤滑層形成工程は、石鹸を含有する潤滑層形成用処理剤を前記皮膜に接触（付着）させて潤滑層を形成する工程である。マグネシウムを含む皮膜に石鹸を含有する潤滑層形成用処理剤を接触（付着）させることにより、石鹸中のアルカリ金属がマグネシウムにイオン置換され、マグネシウム金属石鹸を含む潤滑層が形成される。潤滑層形成用処理剤は、例えば、水溶液である。なお、潤滑層形成工程は、金属材料の塑性加工で行われている、石鹸を含む潤滑剤を用いた公知の潤滑処理工程により行ってもよい。
[Lubricant layer formation process]
The lubricating layer forming step is a step of forming a lubricating layer by bringing a soap-containing lubricating layer forming treatment agent into contact with (adhering to) the film. By contacting (adhering) a treatment agent for forming a lubricating layer containing soap to a coating containing magnesium, the alkali metal in the soap is ion-replaced with magnesium, and a lubricating layer containing magnesium metal soap is formed. The lubricating layer forming treatment agent is, for example, an aqueous solution. Note that the lubricant layer forming step may be performed by a known lubrication treatment step using a lubricant containing soap, which is performed in plastic working of metal materials.
石鹸は特に制限されないが、例えば、炭素数１２～２６程度の脂肪酸（ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキジン酸、ベヘン酸、及びリグノセリン酸などの飽和脂肪酸、パルミトレイン酸、オレイン酸、エライジン酸、リノール酸、リノレン酸、アラキドン酸、エイコサペンタエン酸、及びドコサヘキサエン酸などの不飽和脂肪酸、分枝脂肪酸など）のアルカリ金属塩などが挙げられ、好ましくは炭素数１２～２０の脂肪酸のアルカリ金属塩であり、より好ましくは炭素数１２～１８の脂肪酸のナトリウム塩である。これらは１種用いてもよく、２種以上を併用してもよい。 The soap is not particularly limited, but includes, for example, fatty acids having about 12 to 26 carbon atoms (saturated fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, and lignoceric acid, palmitoleic acid, oleic acid, Examples include alkali metal salts of unsaturated fatty acids such as elaidic acid, linoleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid, and docosahexaenoic acid, branched fatty acids, etc., and preferably alkali metal salts of fatty acids having 12 to 20 carbon atoms. A metal salt, more preferably a sodium salt of a fatty acid having 12 to 18 carbon atoms. These may be used alone or in combination of two or more.
潤滑層形成用処理剤中の石鹸の濃度（２種以上の石鹸を含む場合は合計濃度）は特に制限されないが、潤滑層を十分に形成させる観点から、好ましくは０．０１～１０ｍｏｌ／Ｌ、より好ましくは０．０５～５ｍｏｌ／Ｌ、さらに好ましくは０．１～１ｍｏｌ／Ｌ、特に好ましくは０．１～０．５ｍｏｌ／Ｌである。 The concentration of soap in the treatment agent for forming a lubricant layer (total concentration if two or more soaps are included) is not particularly limited, but from the viewpoint of sufficiently forming a lubricant layer, it is preferably 0.01 to 10 mol/L, More preferably 0.05 to 5 mol/L, still more preferably 0.1 to 1 mol/L, particularly preferably 0.1 to 0.5 mol/L.
潤滑層形成用処理剤を前記皮膜に接触（付着）させて潤滑層を形成する際の温度は特に制限されないが、潤滑層を迅速に形成させる観点から、好ましくは７０～９５℃、より好ましくは７５～９０℃、さらに好ましくは８０～９０℃である。 The temperature at which a lubricant layer is formed by contacting (adhering) the lubricant layer forming treatment agent to the film is not particularly limited, but from the viewpoint of rapidly forming a lubricant layer, it is preferably 70 to 95°C, more preferably The temperature is 75 to 90°C, more preferably 80 to 90°C.
潤滑層形成用処理剤を前記皮膜に接触（付着）させる時間は特に制限されないが、潤滑層を十分に形成させる観点、及び製造効率の観点から、好ましくは３０秒間以上１時間以下、より好ましくは１分間以上３０分間以下、さらに好ましくは２分間以上２０分間以下、特に好ましくは３分間以上１０分間以下である。 The time for contacting (adhering) the lubricant layer forming treatment agent to the film is not particularly limited, but from the viewpoint of sufficiently forming a lubricant layer and from the viewpoint of manufacturing efficiency, it is preferably 30 seconds or more and 1 hour or less, more preferably The duration is 1 minute or more and 30 minutes or less, more preferably 2 minutes or more and 20 minutes or less, particularly preferably 3 minutes or more and 10 minutes or less.
潤滑層形成用処理剤を前記皮膜に接触（付着）させる方法は特に制限されず、例えば、ロールコート法、スピンコート法、スプレー法、及び浸漬法などの公知の方法により行うことができる。 The method of bringing the lubricating layer forming treatment agent into contact with (adhering to) the film is not particularly limited, and can be carried out by any known method such as a roll coating method, a spin coating method, a spray method, and a dipping method.
＜潤滑層含有金属材料の製造方法＞
本発明の潤滑層含有金属材料の製造方法は、カリウム及びナトリウムの少なくとも１種を含むアルカリ成分を含有する金属表面前処理剤を金属材料表面に接触させて前処理する前処理工程、マグネシウム化合物を含有する皮膜形成用処理剤を前処理した金属材料表面に接触させて皮膜を形成する皮膜形成工程、及び石鹸を含有する潤滑層形成用処理剤を前記皮膜に接触させて潤滑層を形成する潤滑層形成工程を含む。
<Method for producing metal material containing lubricating layer>
The method for producing a metal material containing a lubricating layer of the present invention includes a pretreatment step in which a metal surface pretreatment agent containing an alkaline component containing at least one of potassium and sodium is brought into contact with the surface of the metal material, and a magnesium compound is pretreated. A film forming step in which a film-forming treatment agent containing a pretreated metal material surface is brought into contact to form a film, and a lubrication step in which a lubricant layer-forming treatment agent containing soap is brought into contact with the film to form a lubricant layer. Including a layer forming step.
前記のとおり、金属表面前処理剤を金属材料表面に接触（付着）させて前処理することにより、金属材料表面にカリウム及び／又はナトリウムを含む粘土化膜が形成される。当該粘土化膜にマグネシウム化合物を含有する皮膜形成用処理剤を接触（付着）させることにより、当該粘土化膜中のカリウム及び／又はナトリウムがマグネシウムにイオン置換され、マグネシウムを含む皮膜（粘土化膜）が形成される。そして、マグネシウムを含む皮膜に石鹸を含有する潤滑層形成用処理剤を接触（付着）させることにより、石鹸中のアルカリ金属がマグネシウムにイオン置換され、マグネシウム金属石鹸を含む潤滑層が形成される。当該潤滑層は、金属材料表面に強固に付着しているため剥離しにくく、金属材料の塑性加工において優れた潤滑性を発揮する。そのため、本発明の製造方法により得られる潤滑層含有金属材料は、塑性加工性に優れるものである。 As described above, by contacting (adhering) the metal surface pretreatment agent to the surface of the metal material for pretreatment, a clay film containing potassium and/or sodium is formed on the surface of the metal material. By contacting (adhering) a film-forming treatment agent containing a magnesium compound to the clay film, potassium and/or sodium in the clay film is ion-replaced with magnesium, forming a magnesium-containing film (clay film). ) is formed. Then, by contacting (adhering) a treatment agent for forming a lubricating layer containing soap to the film containing magnesium, the alkali metal in the soap is ion-replaced with magnesium, and a lubricating layer containing magnesium metal soap is formed. The lubricating layer is firmly attached to the surface of the metal material, so it is difficult to peel off, and exhibits excellent lubricity during plastic working of the metal material. Therefore, the lubricating layer-containing metal material obtained by the manufacturing method of the present invention has excellent plastic workability.
本発明の潤滑層含有金属材料の製造方法における、前処理工程、皮膜形成工程、及び潤滑層形成工程は、＜金属材料表面への潤滑層形成方法＞の欄に記載したとおりである。 In the method for producing a metal material containing a lubricant layer of the present invention, the pretreatment step, film formation step, and lubricant layer formation step are as described in the section <Method for forming a lubricant layer on the surface of a metal material>.
本発明の潤滑層含有金属材料は、塑性加工性に優れるため、金属材料を塑性加工する金属加工方法に好適に用いられる。前記金属加工方法は、本発明の潤滑層含有金属材料を用いる以外は公知の方法を採用することができる。塑性加工としては、例えば、鍛造、伸線、伸管、ロールフォーミング、及びプレスなどが挙げられる。 Since the lubricating layer-containing metal material of the present invention has excellent plastic workability, it is suitably used in a metal working method for plastic working a metal material. As the metal processing method, a known method can be adopted except for using the lubricating layer-containing metal material of the present invention. Examples of plastic working include forging, wire drawing, tube drawing, roll forming, and pressing.
なお、必須の工程ではないが、金属加工する前に、潤滑層が形成された金属材料表面に潤滑剤を接触（付着）させる潤滑処理を行ってもよい。 Although it is not an essential step, a lubrication process may be performed in which a lubricant is brought into contact with (adhered to) the surface of the metal material on which a lubricant layer is formed before metal processing.
潤滑処理の方法としては、金属材料の塑性加工で行われている、公知の潤滑処理の方法が採用できる。潤滑処理において、潤滑剤の潤滑剤成分としては、例えば、二硫化モリブデンやグラファイトなどの固体潤滑剤、油、及び石鹸などが挙げられる。潤滑剤成分は、１種類のみを用いてもよいし、２種類以上を混合して用いてもよい。 As the lubrication treatment method, a known lubrication treatment method used in plastic working of metal materials can be adopted. In the lubrication process, lubricant components of the lubricant include, for example, solid lubricants such as molybdenum disulfide and graphite, oil, and soap. Only one type of lubricant component may be used, or a mixture of two or more types may be used.
油としては、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキヂン酸、ベヘン酸、リグノセリン酸などの飽和脂肪酸、パルミトレイン酸、オレイン酸、エライジン酸、リノール酸、リノレン酸、アラキドン酸、エイコサペンタエン酸、ドコサヘキサエン酸等の不飽和脂肪酸、分枝脂肪酸などの、炭素数１２～２６程度の脂肪酸が挙げられる。また、石鹸としては、炭素数１２～２６程度の脂肪酸（ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキヂン酸、ベヘン酸、リグノセリン酸などの飽和脂肪酸、パルミトレイン酸、オレイン酸、エライジン酸、リノール酸、リノレン酸、アラキドン酸、エイコサペンタエン酸、ドコサヘキサエン酸等の不飽和脂肪酸、分枝脂肪酸など）のアルカリ金属塩、もしくは、炭素数１２～２６の脂肪酸（ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキヂン酸、ベヘン酸、リグノセリン酸などの飽和脂肪酸、パルミトレイン酸、オレイン酸、エライジン酸、リノール酸、リノレン酸、アラキドン酸、エイコサペンタエン酸、ドコサヘキサエン酸等の不飽和脂肪酸、分枝脂肪酸など）と、亜鉛、カルシウム、バリウム、アルミニウム、及びマグネシウムから選ばれる少なくとも１種の金属とを反応させて得られた金属石鹸などが挙げられる。 Oils include saturated fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, and lignoceric acid, palmitoleic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, arachidonic acid, and eicosapentaenoic acid. , unsaturated fatty acids such as docosahexaenoic acid, and branched fatty acids having about 12 to 26 carbon atoms. In addition, soaps include fatty acids with about 12 to 26 carbon atoms (saturated fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, lignoceric acid, palmitoleic acid, oleic acid, elaidic acid, linoleic acid, etc.). acids, alkali metal salts of unsaturated fatty acids such as linolenic acid, arachidonic acid, eicosapentaenoic acid, docosahexaenoic acid, branched fatty acids, etc.), or fatty acids with 12 to 26 carbon atoms (lauric acid, myristic acid, palmitic acid, stearic acid, etc.). saturated fatty acids such as arachidic acid, behenic acid, lignoceric acid, unsaturated fatty acids such as palmitoleic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid, docosahexaenoic acid, branched fatty acids, etc.) Examples include metal soaps obtained by reacting with at least one metal selected from zinc, calcium, barium, aluminum, and magnesium.
潤滑剤は、前記潤滑剤成分を含む水溶液の形態で使用することができる。水溶液中の潤滑剤成分の濃度は、所定量の潤滑剤成分が金属材料表面に付着すれば特に制限されないが、例えば、０．５～１０質量％程度である。 The lubricant can be used in the form of an aqueous solution containing the lubricant components. The concentration of the lubricant component in the aqueous solution is not particularly limited as long as a predetermined amount of the lubricant component adheres to the surface of the metal material, but is, for example, about 0.5 to 10% by mass.
潤滑処理における温度は特に制限されず、金属材料表面についての公知の潤滑処理の条件を採用することができ、例えば、３０～１００℃程度、好ましくは４０～９０℃、より好ましくは６０～９０℃である。 The temperature in the lubrication treatment is not particularly limited, and any known lubrication treatment conditions for metal material surfaces can be adopted, for example, about 30 to 100°C, preferably 40 to 90°C, more preferably 60 to 90°C. It is.
以下に、実施例及び比較例を示して本発明を詳細に説明する。ただし、本発明は、実施例に限定されない。 The present invention will be explained in detail below by showing Examples and Comparative Examples. However, the present invention is not limited to the examples.
［実施例１～８及び比較例２～３］
１．処理剤の調製
以下のようにして、金属表面前処理剤、皮膜形成用処理剤、及び潤滑層形成用処理剤をそれぞれ調製した。
[Examples 1 to 8 and Comparative Examples 2 to 3]
1. Preparation of Treatment Agents A metal surface pretreatment agent, a film formation treatment agent, and a lubricant layer formation treatment agent were each prepared as follows.
＜金属表面前処理剤＞
実施例１～４および実施例７～８においては、市販の水酸化ナトリウム、実施例５～６においては、市販の水酸化カリウム、比較例２～３においては、市販の水酸化マグネシウムを、それぞれ、アルカリ成分とした。各アルカリ成分を、それぞれ、表１の「金属表面前処理剤」の欄に記載の濃度（Ｍ＝ｍｏｌ／Ｌ）になるようにして、水に溶解または懸濁し、金属表面前処理剤を得た。
<Metal surface pretreatment agent>
In Examples 1 to 4 and Examples 7 to 8, commercially available sodium hydroxide, in Examples 5 to 6, commercially available potassium hydroxide, and in Comparative Examples 2 to 3, commercially available magnesium hydroxide, respectively. , as an alkaline component. Each alkali component was dissolved or suspended in water to the concentration (M = mol/L) listed in the "Metal surface pretreatment agent" column of Table 1 to obtain a metal surface pretreatment agent. Ta.
＜皮膜形成用処理剤＞
実施例１～８において、皮膜形成用処理剤は、市販の塩化マグネシウム六水和物を、表１の「皮膜形成用処理剤」の欄に示す濃度（Ｍ＝ｍｏｌ／Ｌ）になるようにして水に溶解して、アンモニウム水でｐＨ９．５に調整することで調製した。
<Film forming treatment agent>
In Examples 1 to 8, the film-forming treatment agent was commercially available magnesium chloride hexahydrate at a concentration (M = mol/L) shown in the "Film-forming treatment agent" column of Table 1. It was prepared by dissolving it in water and adjusting the pH to 9.5 with ammonium water.
＜潤滑層形成用処理剤＞
実施例１～８においては、潤滑層形成用処理剤として、表１の「石鹸を含有する水溶液」の欄に記載の各石鹸を０．１（Ｍ＝ｍｏｌ／Ｌ）の濃度で含む水溶液を用いた。比較例２～３においては、潤滑処理剤として、表１の「石鹸を含有する水溶液」の欄に記載の各石鹸を０．１（Ｍ＝ｍｏｌ／Ｌ）の濃度で含む水溶液を用いた。
<Treatment agent for forming lubricating layer>
In Examples 1 to 8, an aqueous solution containing each soap listed in the "Aqueous solution containing soap" column of Table 1 at a concentration of 0.1 (M = mol/L) was used as a treatment agent for forming a lubricating layer. Using. In Comparative Examples 2 and 3, an aqueous solution containing each soap listed in the "Soap-containing aqueous solution" column of Table 1 at a concentration of 0.1 (M=mol/L) was used as the lubricant.
［実施例１～８］
２．金属材料の表面処理
＜前処理工程＞
アルミニウム材（それぞれ、後述の試験に供した、Ａ５０５２材（リング）およびＡ５０５６材（後方押出し）を、表１に記載の各金属表面前処理剤に４０℃で３分間浸漬した後、水洗した。
[Examples 1 to 8]
2. Surface treatment of metal materials <pretreatment process>
Aluminum materials (A5052 material (ring) and A5056 material (backward extrusion), each subjected to the test described below) were immersed in each metal surface pretreatment agent listed in Table 1 at 40° C. for 3 minutes, and then washed with water.
＜皮膜形成工程＞
前処理工程の後、各アルミニウム材を、表１に記載の各皮膜形成用処理剤に８５℃で５分間浸漬して、前処理工程で付着させたアルカリ成分のアルカリ金属とマグネシウムとの置換反応により、各アルミニウム材の表面に、マグネシウムを含む皮膜（層状複水酸化物の粘土化膜）を形成した。
<Film formation process>
After the pre-treatment process, each aluminum material was immersed in each film-forming treatment agent listed in Table 1 at 85°C for 5 minutes to undergo a substitution reaction between the alkali metal and magnesium in the alkali component deposited in the pre-treatment process. As a result, a film containing magnesium (layered double hydroxide clay film) was formed on the surface of each aluminum material.
＜潤滑層形成工程＞
皮膜形成工程の後、各アルミニウム材を、表１に記載の各石鹸を含有する水溶液に８５℃で５分間浸漬した後、室温で水溶液を乾燥させて、アルミニウム材の表面にマグネシウム金属石鹸を含有する潤滑層を形成した。
<Lubricant layer formation process>
After the film forming step, each aluminum material was immersed in an aqueous solution containing each soap listed in Table 1 at 85°C for 5 minutes, and then the aqueous solution was dried at room temperature to form a layer containing magnesium metal soap on the surface of the aluminum material. A lubricating layer was formed.
［比較例２～３］
２．金属材料の表面処理
＜前処理工程＞
アルミニウム材（それぞれ、後述の試験に供した、Ａ５０５２材（リング）およびＡ５０５６材（後方押出し）を、表１に記載の各金属表面前処理剤に４０℃で３分間浸漬した後、水洗した。
[Comparative Examples 2-3]
2. Surface treatment of metal materials <pretreatment process>
Aluminum materials (A5052 material (ring) and A5056 material (backward extrusion), each subjected to the test described below) were immersed in each metal surface pretreatment agent listed in Table 1 at 40° C. for 3 minutes, and then washed with water.
＜潤滑処理工程＞
前処理工程の後、各アルミニウム材を、表１に記載の各石鹸を含有する水溶液に８５℃で５分間浸漬した後、室温で水溶液を乾燥させて、アルミニウム材の表面に石鹸を付着させた。
<Lubrication process>
After the pretreatment step, each aluminum material was immersed in an aqueous solution containing each soap listed in Table 1 at 85°C for 5 minutes, and then the aqueous solution was dried at room temperature to adhere the soap to the surface of the aluminum material. .
［比較例１］
アルミニウム材をフッ化アルミ亜鉛処理法で表面に金属表面前処理剤の塗膜を形成し、貴和化学薬品製「フェロリューベＮｏ．１」の３％水溶液を用いて潤滑処理し、室温で、潤滑膜を乾燥させて、潤滑剤を付着させたアルミニウム材を得た。
[Comparative example 1]
A coating film of a metal surface pretreatment agent was formed on the surface of the aluminum material using the aluminum zinc fluoride treatment method, and the material was lubricated using a 3% aqueous solution of ``Ferrolube No. 1'' manufactured by Kiwa Chemicals, and then treated at room temperature. The lubricant film was dried to obtain an aluminum material to which the lubricant was attached.
３．金属材料の塑性加工性の評価
実施例１～８で得られた潤滑層を有するアルミニウム材、及び比較例１～３で得られた表面処理したアルミニウム材について、それぞれ、以下のリンク圧縮試験、及び後方押出し試験を行い、金属材料の塑性加工性を評価した。結果を表２に示す。
3. Evaluation of plastic workability of metal materials The aluminum materials with a lubricating layer obtained in Examples 1 to 8 and the surface-treated aluminum materials obtained in Comparative Examples 1 to 3 were subjected to the following link compression test and A backward extrusion test was conducted to evaluate the plastic workability of the metal material. The results are shown in Table 2.
＜リング圧縮試験＞
リング圧縮試験に用いたリングの材質は、アルミニウムＡ５０５２材であり、外径は２１．０ｍｍ、内径は１０．５ｍｍ、厚みは７．０ｍｍのものを用いた。実施例１～８で得られた潤滑層を有するアルミニウム材、及び比較例１～３で得られた表面処理したアルミニウム材からなる各リングを２００トンの荷重、圧縮率が６０％でプレスした。圧縮後のリングの厚み、及び内径を測定し、摩擦係数を測定した。なお、それぞれ３回ずつリング圧縮試験を行い、平均の摩擦係数μを求めた。なお、リング圧縮試験において、リングは圧縮される時の圧縮後の形状と摩擦係数との関係は知られている。摩擦係数が小さい場合は、内径・外径とも外側に張り出すように圧縮される。また、摩擦係数が大きい場合は、内径は内側に張り出し、外径も外側に張り出す長さが小さくなる。故に、内径部の寸法変化を測定し、摩擦係数の算出を行うことができる。摩擦係数が低いほど、潤滑性能が高い。一般に、現在広く使用されているフッ化アルミ亜鉛処理法での摩擦係数より低ければ使用可能とされる。
<Ring compression test>
The material of the ring used in the ring compression test was aluminum A5052 material, and had an outer diameter of 21.0 mm, an inner diameter of 10.5 mm, and a thickness of 7.0 mm. Each ring made of the aluminum material having a lubricating layer obtained in Examples 1 to 8 and the surface-treated aluminum material obtained in Comparative Examples 1 to 3 was pressed at a load of 200 tons and a compression ratio of 60%. The thickness and inner diameter of the ring after compression were measured, and the coefficient of friction was measured. The ring compression test was performed three times for each sample, and the average friction coefficient μ was determined. In the ring compression test, the relationship between the shape of the ring after compression and the friction coefficient is known. When the coefficient of friction is small, both the inner and outer diameters are compressed so as to bulge outward. Further, when the coefficient of friction is large, the inner diameter protrudes inward, and the length in which the outer diameter protrudes outward becomes smaller. Therefore, the dimensional change of the inner diameter portion can be measured and the coefficient of friction can be calculated. The lower the friction coefficient, the higher the lubrication performance. Generally, it can be used if the friction coefficient is lower than that of the aluminum zinc fluoride treatment method that is currently widely used.
＜後方押出し試験＞
後方押出し試験に用いた円柱試験片の材質は、アルミニウムＡ５０５６材であり、直径は２９．９ｍｍ、高さは２４．０ｍｍのものを用いた。後方押出し試験は次の通りである。まず、金型に、実施例１～８で得られた潤滑層を有するアルミニウム材、及び比較例１～３で得られた表面処理したアルミニウム材からなる各円柱試験片を挿入し、２００トンの荷重、圧縮速度が２０％でプレスした。後方押出し後の試験片の外観を観察して、以下の基準によって評価した。
○：焼き付きがない
×：焼き付きがある
<Backward extrusion test>
The material of the cylindrical test piece used in the backward extrusion test was aluminum A5056 material, and had a diameter of 29.9 mm and a height of 24.0 mm. The backward extrusion test is as follows. First, each cylindrical test piece made of the aluminum material with a lubricating layer obtained in Examples 1 to 8 and the surface-treated aluminum material obtained in Comparative Examples 1 to 3 was inserted into a mold, and a 200-ton test piece was inserted into the mold. Pressing was performed at a load and compression speed of 20%. The appearance of the test piece after backward extrusion was observed and evaluated according to the following criteria.
○: No burn-in ×: There is burn-in
表２に示すように、実施例１～８で得られた潤滑層を有するアルミニウム材は、比較例１～３で得られた表面処理したアルミニウム材に比べて摩擦係数が小さく、また、焼き付きも生じないものであった。これらの結果から、実施例１～８で得られた潤滑層を有するアルミニウム材は、塑性加工性に優れることがわかる。 As shown in Table 2, the aluminum materials with a lubricating layer obtained in Examples 1 to 8 have a smaller coefficient of friction than the surface-treated aluminum materials obtained in Comparative Examples 1 to 3, and are also less likely to seize. It was something that would not happen. These results show that the aluminum materials having the lubricating layer obtained in Examples 1 to 8 have excellent plastic workability.
本発明の潤滑層含有金属材料は、鍛造、伸線、伸管、ロールフォーミング、及びプレスなどの塑性加工に好適に用いられる。 The lubricating layer-containing metal material of the present invention is suitably used for plastic working such as forging, wire drawing, pipe drawing, roll forming, and pressing.
Claims (9)
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