CN114134500A - 一种镁锂合金蒙皮表面结合力提升处理方法 - Google Patents
一种镁锂合金蒙皮表面结合力提升处理方法 Download PDFInfo
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- 229910000733 Li alloy Inorganic materials 0.000 title claims abstract description 106
- 239000001989 lithium alloy Substances 0.000 title claims abstract description 106
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000126 substance Substances 0.000 claims abstract description 37
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000007739 conversion coating Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 91
- 238000000576 coating method Methods 0.000 claims description 47
- 239000011248 coating agent Substances 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 36
- 239000011259 mixed solution Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 21
- 238000001723 curing Methods 0.000 claims description 18
- 150000004703 alkoxides Chemical class 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007822 coupling agent Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 230000001680 brushing effect Effects 0.000 claims description 6
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- 150000001282 organosilanes Chemical class 0.000 claims description 3
- 125000005375 organosiloxane group Chemical group 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 4
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- 229910052757 nitrogen Inorganic materials 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 229960001124 trientine Drugs 0.000 description 4
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910002801 Si–O–Mg Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- PDRQZRNOXMTBLB-UHFFFAOYSA-N butan-1-ol;hafnium Chemical compound [Hf].CCCCO PDRQZRNOXMTBLB-UHFFFAOYSA-N 0.000 description 1
- SKFIUGUKJUULEM-UHFFFAOYSA-N butan-1-ol;zirconium Chemical compound [Zr].CCCCO SKFIUGUKJUULEM-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- YAXGCGGUIRGMGP-UHFFFAOYSA-N hafnium;propan-1-ol Chemical compound [Hf].CCCO YAXGCGGUIRGMGP-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- NSATXMGEEXXFTR-UHFFFAOYSA-N propan-1-ol;yttrium Chemical compound [Y].CCCO NSATXMGEEXXFTR-UHFFFAOYSA-N 0.000 description 1
- RQIHICWHMWNVSA-UHFFFAOYSA-N propan-1-ol;zirconium Chemical compound [Zr].CCCO RQIHICWHMWNVSA-UHFFFAOYSA-N 0.000 description 1
- FXWGWZQOSOJYOC-UHFFFAOYSA-N propane-1,2,3-triol;titanium Chemical compound [Ti].OCC(O)CO FXWGWZQOSOJYOC-UHFFFAOYSA-N 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
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Abstract
一种镁锂合金蒙皮表面结合力提升处理方法,在镁锂合金表面制备化学转化‑溶胶凝胶复合膜层,具体制备步骤如下:对镁锂合金材料表面进行碱洗,碱洗完成后将镁锂合金蒙皮从溶液中取出;将镁锂合金蒙皮表面上残留的溶液用去离子水清洗;对镁锂合金蒙皮表面进行化学转化膜处理,化学转化膜处理完成后将镁锂合金蒙皮从溶液中取出;将生成化学转化膜后的镁锂合金蒙皮表面上残留的溶液用去离子水清洗;将水洗后的镁锂合金蒙皮放入烘箱中热处理;在热处理后的镁铝合金蒙皮表面生成溶胶凝胶膜层。本发明方法采用化学氧化和表面喷涂溶胶凝胶进行前处理,以提高其与热控漆之间的结合力。
Description
技术领域
本发明涉及一种镁锂合金蒙皮表面结合力提升溶胶-凝胶处理方法,属于镁锂合金表面防护技术领域。
背景技术
卫星结构板由金属蒙皮及蜂窝结构组成。目前卫星蒙皮为铝合金材料,根据卫星热控需要,蒙皮外表面喷涂热控漆。鉴于镁锂合金具有低材料密度(1.3-1.5g/cm3),且具有比强度和比刚度高、电磁屏蔽性好、良好的阻尼减振性能、塑性好、良好的耐冲击等特点,采用镁锂合金蒙皮替代传统的铝合金蒙皮,是实现航天器实现结构轻量化、高稳定性的有效手段。
但是,由于镁锂合金活泼的化学性质,导致其与表面涂层结合力较差。在镁锂合金表面喷涂热控漆时出现大面积脱落的现象。亟需研究一种适用于镁锂合金蒙皮的表面结合力提升处理方法,满足卫星结构板热控及高稳定性要求。
发明内容
本发明所要解决的技术问题是:针对镁锂合金蒙皮大型薄壁结构,本发明提供了一种镁锂合金蒙皮表面结合力提升处理方法,采用化学氧化和表面喷涂溶胶凝胶进行前处理,以提高其与热控漆之间的结合力。
本发明所采用的技术方案如下:一种镁锂合金蒙皮表面结合力提升处理方法,在镁锂合金表面制备化学转化-溶胶凝胶复合膜层,具体制备步骤如下:
对镁锂合金材料表面进行碱洗,碱洗完成后将镁锂合金蒙皮从溶液中取出;
将镁锂合金蒙皮表面上残留的溶液用去离子水清洗;
对镁锂合金蒙皮表面进行化学转化膜处理,化学转化膜处理完成后将镁锂合金蒙皮从溶液中取出;
将生成化学转化膜后的镁锂合金蒙皮表面上残留的溶液用去离子水清洗;
将水洗后的镁锂合金蒙皮放入烘箱中热处理;
在热处理后的镁铝合金蒙皮表面生成溶胶凝胶膜层。
碱洗溶液中包含氢氧化钠30g/L~50g/L、磷酸钠8g/L~12g/L;碱洗的温度为60℃~90℃,时间为5min~10min。
化学转化膜处理中使用的溶液中包括氟化钠20~30g/L、氢氟酸2g/L~3g/L;化学转化膜处理过程中温度为20℃~30℃,处理时间为10s~20s。
热处理的温度为80~100℃,热处理时间为2h。
溶胶凝胶膜层的具体制备步骤包含配置溶胶,在生成化学转化膜的镁铝合金蒙皮表面涂覆溶胶,进行干燥固化。
配制溶胶包括步骤如下:
步骤6.1、配置改性硅溶胶包括:
配置含氨基的有机硅烷和醇的混合溶液,其中,有机硅氧烷与醇的体积比例为1:2~2:1;
在设定的温度和速率搅拌条件下,将去离子水加入混合溶液中,并进行持续搅拌2h,去离子水和混合溶液的体积比为1:5~1:8,,搅拌温度为5℃~60℃;搅拌速率为100~400r/min;
步骤6.2、配制金属醇盐溶胶包括:
配制醇和水的混合溶液,其中,水采用去离子水,醇和水的体积比比例为5:1~10:1
在设定的温度和速率搅拌条件下,将催化剂加入醇和水的混合溶液,并进行持续搅拌;所加入催化剂与醇水溶剂体积比为2:1~7:1,搅拌温度为5℃~60℃;搅拌速率为100r/min~400r/min;搅拌时间为5min~10min;
在设定的温度和速率搅拌条件下,将金属醇盐缓慢倒入混合溶液中,并进行持续搅拌;所加入的金属醇盐与混合溶液体积比为0.5:1~2:1;搅拌温度为5℃~60℃;搅拌速度为300r/min~800r/min;搅拌时间为0.5h~6h;
步骤6.3、制备有机-无机杂化溶胶包括:
将步骤6.2配制的的金属醇盐溶胶缓慢加入到步骤6.1配制的硅溶胶中,并进行持续搅拌;所加入的金属醇盐溶胶与硅溶胶体积比为1:10~1:2;搅拌温度为5℃~60℃;搅拌速度为400~1000r/min,;搅拌时间为0.5h~3h;
在设定的温度和速率搅拌条件下,将碱性偶联剂加入混合溶胶中,并进行持续搅拌;所加入的碱性偶联剂与混合溶胶质量比为0.1wt.%~0.5wt.%,搅拌温度为5℃~60℃;搅拌速率为400r/min~1000r/min;搅拌时间为0.5h~3h。
在生成化学转化膜的镁铝合金蒙皮表面涂覆溶胶包括:
采用喷涂法或涂刷法制备膜层,膜层厚度控制在0.5μm~20μm之间;涂覆次数控制在1次~3次之间,每次涂覆之间间隔10min~15min。
干燥固化的步骤如下:
涂覆后的镁锂合金蒙皮首先在室温下自然干燥10min~30min,待溶胶充分平整,随后将镁锂合金蒙皮放置于空气炉中加热至70℃~120℃,固化1h~10h,然后随炉冷却至室温,取出镁锂合金蒙皮。
干燥固化时,固化温度优选80℃~110℃;固化时间优选2h~8h。
本发明与现有技术相比的有益效果是:
(1)本发明在镁锂合金表面制备氟化镁化学转化膜可以起到防止腐蚀点产生及腐蚀修复的功能,可显著提高镁锂合金的防腐性能,同时其表面为粗糙的多孔结构,有利于其与后续溶胶凝胶膜层的结合力,为复合膜层的制备奠定基础。
(2)本发明制备的溶胶凝胶膜层水解生成硅醇后与镁锂合金基材表面氧化物形成Si-O-Mg的化学键,从而实现与氧化膜的化学键合,提高膜层结合力,同时由于过渡层的覆盖,填补了氧化膜的空隙,同时隔绝了氧化膜与空气的接触,从而有效提高了膜层的防腐性能。另一方面,溶胶凝胶中的乙氧基与热控涂层树脂中的羟基发生缩聚反应形成Si-O-Si化学键;溶胶凝胶中的氨基还可在室温条件可以与树脂的环氧基团发生加成反应,以此提高溶胶凝胶膜层与后续热控涂层的结合力。
(3)本发明制备的溶胶凝胶膜层采用有机缓释剂改性碱性有机-无机杂化溶胶凝胶体系,利用硅烷偶联剂本身的碱性进行水解-缩合反应形成有机-无机杂化溶胶,同时添加碱性的偶联剂提高其与基材和热控涂层的结合力。避免传统质子酸催化剂的添加造成镁锂合金的腐蚀,适用于性质活泼的镁锂合金表面。
(4)采用本发明所述一种镁锂合金蒙皮表面结合力提升处理方法,在喷涂SR107和E51-M热控涂层后,按照GB/T 9286-1998《色漆和清漆漆膜的划格试验》规定的方法进行划格法结合力测试,热控涂层结合力均大于1级。
(5)采用本发明所述一种镁锂合金蒙皮表面结合力提升处理方法,在喷涂SR107和E51-M热控涂层后,按照GJB2502.8《航天器热控涂层试验方法第8部分:热循环试验》的规定的方法进行涂层的常压热循环试验,涂层经100次-196℃(液氮,5min)~100℃(5min)的热循环试验后,涂层外观完好,无起泡、起皮、开裂、脱落等现象。
附图说明
图1为本发明的方法流程图。
具体实施方式
以下结合实施例对本发明作进一步说明。
如图1所示,一种镁锂合金蒙皮表面结合力提升处理方法,在镁锂合金表面制备化学转化-溶胶凝胶复合膜层。
化学转化膜层,其具体制备步骤包括镁锂合金碱洗、水洗、化学转化膜生成、水洗、热处理五部分。
(1)对镁锂合金材料表面进行前处理,碱洗溶液配方及操作条件如下:
碱洗完成后将镁锂合金从溶液中取出;
(2)将步骤(1)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(3)将步骤(2)得到的镁锂合金材料表面进行化学转化膜处理,溶液配方及操作条件如下:
化学转化膜处理完成后将镁锂合金从溶液中取出;
(4)将步骤(3)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(5)将步骤(4)镁锂合金材料放入烘箱中热处理,热处理温度为80~100℃,热处理时间为2h。
溶胶凝胶膜层,其具体制备步骤包含溶胶配置、溶胶涂覆、干燥固化三个部分。
(1)溶胶配制
I.改性硅溶胶的配置:
①配置含氨基的有机硅烷(选自KH550、KBM603、KBM-602、Y-5691等,或其混合物)和醇(选自甲醇、乙醇、乙二醇、正丙醇,等)的混合溶液,其中有机硅氧烷与醇的体积比例为1:2~2:1,优选1:1;
②在一定温度和速率搅拌条件下,将去离子水加入步骤①配置的混合溶液中,并进行持续搅拌2h,去离子水和混合溶液的体积比为1:5~1:8,优选1:6~1:7,搅拌温度维持5℃~60℃,优选15℃~50℃;搅拌速率维持100~400r/min,优选200~300r/min;
III.金属醇盐溶胶的配制:
①配制醇和水的混合溶液,其中醇(选自甲醇、乙醇、乙二醇、正丙醇等),水采用去离子水,醇和水的体积比比例为5:1~10:1,优选8:1~10:1;
②在一定温度和速率搅拌条件下,将催化剂(选自乙酰丙酮、乙酰乙酸乙酯等)加入醇和水的混合溶液,并进行持续搅拌;所加入催化剂与醇水溶剂体积比为2:1~7:1,优选体积比为3:1~4:1搅拌温度维持5℃~60℃,优选15℃~50℃;搅拌速率维持100r/min~400r/min,优选200r/min~300r/min;搅拌时间维持5min~10min;
③在一定温度和速率搅拌条件下,将金属醇盐(选自钛酸四正丁酯、钛酸四正丁酯、丙三醇钛、丙醇锆、正丙醇锆、正丁醇锆、丙醇铪、正丁醇铪、正丙醇钇等)缓慢倒入上述混合溶液,并进行持续搅拌;所加入金属醇盐与混合溶液体积比为0.5:1~2:1,优选体积比为1:1~2:1;搅拌温度维持5℃~60℃,优选15℃~50℃;搅拌速度维持300r/min~800r/min,优选400r/min~500r/min;搅拌时间维持0.5h~6h,优选1~4h;
IV.有机-无机杂化溶胶制备及改性
①将搅拌时间相同的金属醇盐溶胶缓慢加入硅溶胶,并进行持续搅拌;所加入金属醇盐溶胶与硅溶胶体积比为1:10~1:2,优选体积比为1:8~1:4;搅拌温度维持5℃~60℃,优选15℃~50℃;搅拌速度维持400~1000r/min,优选500~700r/min;搅拌时间维持0.5h~3h,优选1~2h;
②在一定温度和速率搅拌条件下,将碱性偶联剂(三乙烯四胺、乙二胺等)加入上述混合溶胶,并进行持续搅拌;所加入碱性偶联剂与混合溶胶质量比为0.1wt.%~0.5wt.%,搅拌温度维持5℃~60℃,优选15℃~30℃;搅拌速率维持400r/min~1000r/min,优选500r/min~700r/min;搅拌时间维持0.5h~3h,优选1h~2h。
(2)溶胶涂覆
采用喷涂法或涂刷法制备膜层,膜层厚度根据实际需要控制在0.5μm~20μm之间;涂覆次数实际需要控制在1次~3次之间,每次涂覆之间间隔10min~15min。
(3)干燥固化
涂覆后的金属试片首先在室温下自然干燥10min~30min待溶胶充分平整,随后将其放置于空气炉中加热至70℃~120℃固化1h~10h,然后随炉冷却至室温,取出试片;固化温度优选80℃~110℃;固化时间优选2h~8h。
实施例1:
一种镁锂合金蒙皮表面结合力提升处理方法,包括步骤如下:
(1)对镁锂合金材料表面进行前处理,碱洗溶液配方及操作条件如下:
碱洗完成后将镁锂合金从溶液中取出;
(2)将步骤(1)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(3)将步骤(2)得到的镁锂合金材料表面进行化学转化膜处理,溶液配方及操作条件如下:
完成后将镁锂合金从溶液中取出;
(4)将步骤(3)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(5)将步骤(4)镁锂合金材料放入烘箱中热处理,热处理温度为100℃,热处理时间为2h。
(6)溶胶配制
将170ml无水乙醇和170ml KH550倒入烧杯中进行混合,室温下以200r/min速率搅拌均匀;将68ml去离子水缓慢倒入上述混合溶液,以原设定速率继续搅拌2h,得到硅溶胶。
将10ml无水乙醇、2mL去离子水和36ml乙酰丙酮混合,室温下以100r/min速率搅拌均匀;并在搅拌条件下,将48ml正丙醇锆缓慢倒入上述混合溶液,以300r/min速率继续搅拌1h,得到锆溶胶。
将锆溶胶缓慢倒入硅溶胶,室温下500r/min速率搅拌2h;将0.05g三乙烯四胺加入上述混合溶液中,以原设定速率继续搅拌2h,得到所需溶胶。
(7)溶胶涂覆
采用涂刷法制备膜层,膜层厚度控制在0.5μm,涂覆1次。
(8)干燥固化
涂覆后的镁锂合金试样室温下干燥10min,随后将其放置于空气炉中80℃加热2h,然后随炉冷却至室温,取出试片。
(9)在化学转化-溶胶凝胶复合处理后的镁锂合金表面喷涂SR107白漆,采用划格法测试结合力,涂层无任何起皮现象,涂层结合力均达到0级,满足GB/T 9286-1998标准优于1级的要求。涂层经100次-196℃(液氮,5min)~100℃(5min)的热循环试验后,涂层外观完好,无起泡、起皮、开裂、脱落等现象。
实施例2:
一种镁锂合金蒙皮表面结合力提升处理方法,包括步骤如下:
(1)对镁锂合金材料表面进行前处理,碱洗溶液配方及操作条件如下:
碱洗完成后将镁锂合金从溶液中取出;
(2)将步骤(1)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(3)将步骤(2)得到的镁锂合金材料表面进行化学转化膜处理,溶液配方及操作条件如下:
完成后将镁锂合金从溶液中取出;
(4)将步骤(3)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(5)将步骤(4)镁锂合金材料放入烘箱中热处理,热处理温度为100℃,热处理时间为2h。
(6)溶胶配制
将170ml无水乙醇和170ml KH550倒入烧杯中进行混合,室温下以400r/min速率搅拌均匀;将42.5ml去离子水缓慢倒入上述混合溶液,以原设定速率继续搅拌2h,得到硅溶胶。
将10ml无水乙醇、1ml去离子水和77ml乙酰丙酮混合,室温下以200r/min速率搅拌均匀;并在搅拌条件下,将176ml正丙醇锆缓慢倒入上述混合溶液,以800r/min速率继续搅拌4h,得到锆溶胶。
将锆溶胶缓慢倒入硅溶胶,60℃温度下700r/min速率搅拌2h;将0.2g三乙烯四胺加入上述混合溶液中,以原设定速率继续搅拌2h,得到所需溶胶。
(7)溶胶涂覆
采用涂刷法制备膜层,膜层厚度控制在20μm,涂覆3次,两次涂覆间隔10min。
(8)干燥固化
涂覆后的镁锂合金试样室温下干燥30min,随后将其放置于空气炉中120℃加热10h,然后随炉冷却至室温,取出试片。
(9)在化学转化-溶胶凝胶复合处理后的镁锂合金表面喷涂SR107白漆,采用划格法测试结合力,涂层无任何起皮现象,涂层结合力均达到0级,满足GB/T 9286-1998标准优于1级的要求。涂层经100次-196℃(液氮,5min)~100℃(5min)的热循环试验后,涂层外观完好,无起泡、起皮、开裂、脱落等现象。
实施例3:
一种镁锂合金蒙皮表面结合力提升处理方法,包括步骤如下:
(1)对镁锂合金材料表面进行前处理,碱洗溶液配方及操作条件如下:
碱洗完成后将镁锂合金从溶液中取出;
(2)将步骤(1)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(3)将步骤(2)得到的镁锂合金材料表面进行化学转化膜处理,溶液配方及操作条件如下:
完成后将镁锂合金从溶液中取出;
(4)将步骤(3)得到的镁锂合金材料表面上残留的溶液用去离子水清洗;
(5)将步骤(4)镁锂合金材料放入烘箱中热处理,热处理温度为100℃,热处理时间为2h。
(6)溶胶配制
将170ml无水乙醇和170mlKH550倒入烧杯中进行混合,室温下以200r/min速率搅拌均匀;将50ml去离子水缓慢倒入上述混合溶液,以原设定速率继续搅拌2h,得到硅溶胶。
将10ml无水乙醇、2mL去离子水和50ml乙酰丙酮混合,室温下以200r/min速率搅拌均匀;并在搅拌条件下,将70ml正丙醇锆缓慢倒入上述混合溶液,以300r/min速率继续搅拌2h,得到锆溶胶。
将锆溶胶缓慢倒入硅溶胶,室温下500r/min速率搅拌2h;将0.1g三乙烯四胺加入上述混合溶液中,以原设定速率继续搅拌2h,得到所需溶胶。
(7)溶胶涂覆
采用涂刷法制备膜层,膜层厚度控制在10μm,涂覆2次,两次涂覆间隔10min。
(8)干燥固化
涂覆后的镁锂合金试样室温下干燥30min,随后将其放置于空气炉中80℃加热2h,然后随炉冷却至室温,取出试片。
(9)在化学转化-溶胶凝胶复合处理后的镁锂合金表面喷涂SR107白漆,采用划格法测试结合力,涂层无任何起皮现象,涂层结合力均达到0级,满足GB/T 9286-1998标准优于1级的要求。涂层经100次-196℃(液氮,5min)~100℃(5min)的热循环试验后,涂层外观完好,无起泡、起皮、开裂、脱落等现象。
本发明未详细说明部分属于本领域技术人员公知技术。
Claims (9)
1.一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,在镁锂合金表面制备化学转化-溶胶凝胶复合膜层,具体制备步骤如下:
对镁锂合金材料表面进行碱洗,碱洗完成后将镁锂合金蒙皮从溶液中取出;
将镁锂合金蒙皮表面上残留的溶液用去离子水清洗;
对镁锂合金蒙皮表面进行化学转化膜处理,化学转化膜处理完成后将镁锂合金蒙皮从溶液中取出;
将生成化学转化膜后的镁锂合金蒙皮表面上残留的溶液用去离子水清洗;
将水洗后的镁锂合金蒙皮放入烘箱中热处理;
在热处理后的镁铝合金蒙皮表面生成溶胶凝胶膜层。
2.根据权利要求1所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,碱洗溶液中包含氢氧化钠30g/L~50g/L、磷酸钠8g/L~12g/L;碱洗的温度为60℃~90℃,时间为5min~10min。
3.根据权利要求1或2所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,化学转化膜处理中使用的溶液中包括氟化钠20~30g/L、氢氟酸2g/L~3g/L;化学转化膜处理过程中温度为20℃~30℃,处理时间为10s~20s。
4.根据权利要求3所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,热处理的温度为80~100℃,热处理时间为2h。
5.根据权利要求4所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,溶胶凝胶膜层的具体制备步骤包含配置溶胶,在生成化学转化膜的镁铝合金蒙皮表面涂覆溶胶,进行干燥固化。
6.根据权利要求5所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,配制溶胶包括步骤如下:
步骤6.1、配置改性硅溶胶包括:
配置含氨基的有机硅烷和醇的混合溶液,其中,有机硅氧烷与醇的体积比例为1:2~2:1;
在设定的温度和速率搅拌条件下,将去离子水加入混合溶液中,并进行持续搅拌2h,去离子水和混合溶液的体积比为1:5~1:8,,搅拌温度为5℃~60℃;搅拌速率为100~400r/min;
步骤6.2、配制金属醇盐溶胶包括:
配制醇和水的混合溶液,其中,水采用去离子水,醇和水的体积比比例为5:1~10:1
在设定的温度和速率搅拌条件下,将催化剂加入醇和水的混合溶液,并进行持续搅拌;所加入催化剂与醇水溶剂体积比为2:1~7:1,搅拌温度为5℃~60℃;搅拌速率为100r/min~400r/min;搅拌时间为5min~10min;
在设定的温度和速率搅拌条件下,将金属醇盐缓慢倒入混合溶液中,并进行持续搅拌;所加入的金属醇盐与混合溶液体积比为0.5:1~2:1;搅拌温度为5℃~60℃;搅拌速度为300r/min~800r/min;搅拌时间为0.5h~6h;
步骤6.3、制备有机-无机杂化溶胶包括:
将步骤6.2配制的金属醇盐溶胶缓慢加入到步骤6.1配制的硅溶胶中,并进行持续搅拌;所加入的金属醇盐溶胶与硅溶胶体积比为1:10~1:2;搅拌温度为5℃~60℃;搅拌速度为400~1000r/min,;搅拌时间为0.5h~3h;
在设定的温度和速率搅拌条件下,将碱性偶联剂加入混合溶胶中,并进行持续搅拌;所加入的碱性偶联剂与混合溶胶质量比为0.1wt.%~0.5wt.%,搅拌温度为5℃~60℃;搅拌速率为400r/min~1000r/min;搅拌时间为0.5h~3h。
7.根据权利要求6所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,在生成化学转化膜的镁铝合金蒙皮表面涂覆溶胶包括:
采用喷涂法或涂刷法制备膜层,膜层厚度控制在0.5μm~20μm之间;涂覆次数控制在1次~3次之间,每次涂覆之间间隔10min~15min。
8.根据权利要求7所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,干燥固化的步骤如下:
涂覆后的镁锂合金蒙皮首先在室温下自然干燥10min~30min,待溶胶充分平整,随后将镁锂合金蒙皮放置于空气炉中加热至70℃~120℃,固化1h~10h,然后随炉冷却至室温,取出镁锂合金蒙皮。
9.根据权利要求8所述的一种镁锂合金蒙皮表面结合力提升处理方法,其特征在于,干燥固化时,固化温度优选80℃~110℃;固化时间优选2h~8h。
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