CN107523814A - 微弧氧化处理的镁合金上的表面处理方法 - Google Patents
微弧氧化处理的镁合金上的表面处理方法 Download PDFInfo
- Publication number
- CN107523814A CN107523814A CN201710598780.8A CN201710598780A CN107523814A CN 107523814 A CN107523814 A CN 107523814A CN 201710598780 A CN201710598780 A CN 201710598780A CN 107523814 A CN107523814 A CN 107523814A
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- China
- Prior art keywords
- magnesium alloy
- mao
- arc oxidation
- differential arc
- processing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000003647 oxidation Effects 0.000 title claims abstract description 23
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 23
- 238000012545 processing Methods 0.000 title claims description 43
- 238000004381 surface treatment Methods 0.000 title description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001994 activation Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 238000007747 plating Methods 0.000 claims description 5
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 4
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 4
- 229940078494 nickel acetate Drugs 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 244000248349 Citrus limon Species 0.000 claims 1
- 235000005979 Citrus limon Nutrition 0.000 claims 1
- 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 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 235000011083 sodium citrates Nutrition 0.000 claims 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical class [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 16
- 230000008021 deposition Effects 0.000 abstract description 8
- 238000003980 solgel method Methods 0.000 abstract description 7
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 28
- 239000010410 layer Substances 0.000 description 12
- 239000011777 magnesium Substances 0.000 description 12
- 229910052749 magnesium Inorganic materials 0.000 description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 7
- 239000003086 colorant Substances 0.000 description 7
- 229910000077 silane Inorganic materials 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 238000004040 coloring Methods 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
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- -1 fluorine decyl triethoxysilane (perfluorodecyltriethoxysilane) Chemical compound 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
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- 239000002105 nanoparticle Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VBGGLSWSRVDWHB-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(trifluoromethoxy)silane Chemical compound FC(F)(F)O[Si](OC(F)(F)F)(OC(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F VBGGLSWSRVDWHB-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002454 metastable transfer emission spectrometry Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000006884 silylation reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/1644—Composition of the substrate porous substrates
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1889—Multistep pretreatment with use of metal first
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25D11/026—Anodisation with spark discharge
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- C—CHEMISTRY; METALLURGY
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/30—Anodisation of magnesium or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D2202/00—Metallic substrate
- B05D2202/20—Metallic substrate based on light metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249967—Inorganic matrix in void-containing component
- Y10T428/24997—Of metal-containing material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
使用微弧氧化(MAO)方法在镁合金上形成化学和机械性的保护氧化膜。所获得MAO表面在各个方面得到进一步改进，并且描述了其过程。第一，通过形成超疏水性表面而增强了保护，其中水接触角大于140°，这归因于分层的纳米‑微结构。第二，改进了MAO表面的电子性能。具有低至0.05Ω/sq的表面电阻的薄膜是通过在MAO表面上化学镀镍沉积而实现的。第三，黑色是通过MAO样品上的溶胶‑凝胶过程所实现的。
Description
本申请是申请日为2014年11月19日、申请号为201410666132.8、发明名称为“微弧氧化处理的镁合金上的表面处理方法”的申请的分案申请。
相关申请的交叉引用
本申请基于35U.S.C.§119(e)要求美国临时申请61/963,017的权益，该美国临时申请于2013年11月21日提交，并且该美国临时申请通过引用而全部结合在本文中。
技术领域
本发明涉及一种在微弧氧化(MAO)处理的镁(Mg)合金表面上形成功能性的涂层的方法，以改变其表面性质。
背景技术
由于例如轻量化、高强度重量比，良好的电磁屏蔽性质以及可铸性的良好性质，镁合金已经越来越多地应用在笔记本电脑的壳体和移动电话的壳体材料。然而，因为在电动势(electromotive force series)和电位势(galvanic series)两方面序列中的活跃位置，镁合金在大气环境中很快腐蚀，尤其是在潮湿环境中[1]。因此，防腐表面处理对于镁合金产品来说是一个不可缺少的制造过程。
在各种防腐表面处理方法中，微弧氧化(MAO)处理是有前途且有效的，从而将具有较好粘合性的厚陶瓷层形成到基板，这同样是兼顾环保性和高性价比。使用电解液将复合镁基陶瓷层形成在其表面上。然而，制造厂商在一些方面并不满意MAO的表面性能。首先，耐腐蚀性需要进一步增强。其次，MAO处理的表面层是绝热和绝缘的。当MAO过程应用到电子壳体材料时，绝缘性质将影响镁合金的一些性质，包括散热性，导电性，和抗电磁干扰性，尤其是在内表面上。第三，使用者并不满意MAO处理的表面的颜色。经过MAO处理之后，颜色选择是有限的，即不同比例下的灰色。
因此，需要提供一种在MAO处理的镁合金表面上的满意的表面处理方法。
发明内容
鉴于前述的背景技术，本发明的目的是提供一种在MAO处理的镁合金表面上的另一种表面处理方法。
因此，一方面，本发明是一种微弧氧化处理的镁(Mg)合金的处理表面的方法，其包括以下步骤：
a.提供一种MAO处理的镁合金样品；
b.将样品浸入到溶液中；和
c.将步骤(b)的样品进行干燥；
其中，从步骤(c)所获得的已处理样品的表面是超疏水的。
在本发明的示范性实施方式中，步骤(c)之后，已处理样品的表面的水接触角至少为140.4°。在另一个示范性实施方式中，步骤(a)的样品在步骤(b)之前通过NaOH溶液所蚀刻。在另外的示范性实施方式中，该溶液选自于由全氟癸基三甲氧基硅烷(perfluorodecyltrimethoxysilane),正辛基三乙氧基硅烷(triethoxyoctylsilane)和全氟癸基三乙氧基硅烷(perfluorodecyltriethoxysilane)组成的组。
在另一示范性实施方式中，溶液是与硅烷混合的四乙基原硅酸酯，并且步骤(b)和步骤(c)重复两次。
在第二方面中，本发明提供了一种镁合金，其包括5-40μm厚度的镁基陶瓷层；和其上的超疏水涂层，该涂层包括硅烷层，从而该表面具有至少140.4°的水接触角。
在示范性实施方式中，该产品是通过发明内容部分的第2到7段中所述的过程而进行制造。在另一示范性实施方式中，合金表面包括鳞片状结构，并且鳞片状结构的薄片具有100到200nm的长度。
在示范性实施方式中，该产品是通过在发明内容部分的第2到6段以及第8段中所述的过程而制造。在另一示范性实施方式中，该表面包括具有200nm大小的纳米颗粒。
在第三方面中，本发明提供了一种处理微弧氧化处理的镁合金的表面的方法，包括：
a.提供微弧氧化处理的镁合金样品；
b.在乙醇溶液中利用醋酸镍溶液预处理该样品；
c.通过还原剂溶液而活化该已预处理样品；以及
d.通过沉积溶液将化学镀镍(electro-less Ni)形成在已活化的样品的表面上。
其中，从步骤(d)获得的已处理样品是导电的。
在示范性实施方式中，还原剂溶液是NaBH4乙醇溶液。在另一示范性实施方式中，沉积溶液包括NiSO4·6H2O、NaH2PO2·H2O、柠檬酸钠、H3BO3、C3H6O3以及硫脲。在另一示范性实施方式中，从步骤(d)获得的已处理样品的表面电阻小于0.05Ω/sq，并且通过四点探针测试法进行测量。
在第四方面中，本发明提供了镁合金，其包括在合金上的10-30μm厚度的镍层，在其之间的微弧氧化处理层的厚度为5-40μm。该镍层在微弧氧化处理层上形成均匀表面，以提供改善的导电性，从而合金具有小于0.05Ω/sq的表面电阻。
在一个示范性实施方式中，微弧氧化处理层具有一些气孔，其具有由镍填充的1-3μm的平均孔径。在另一示范性实施方式中，产品是通过第三方面中的过程所制造。
在第五方面中，本发明提供了一种微弧氧化处理的镁合金表面的处理方法，其包括：
a.提供微弧氧化处理的镁合金样品；
b.将样品浸入到硅烷溶液中；
c.将步骤(b)的样品进行干燥；以及
d.对步骤(c)的样品进行退火；
其中，该溶液是与硅烷相混合的四乙基原硅酸酯，并且步骤(b)和步骤(c)重复三次以上，其中，表面的颜色与标准颜色代码PANTONE 19-0303匹配。
在第六方面，本发明提供了一种镁合金，其包括5-40μm厚度的镁基陶瓷层，和在其上的硅烷涂层，其中该合金的表面颜色与标准颜色代码PANTONE 19-0303相匹配。在示范性实施方式中，镁合金是通过第五方面的过程所制造的。
附图说明
图1(a)和(b)示出了在化学蚀刻过程中形成在MAO处理表面上的纳米结构和其水接触角。
图2(a)和(b)示出了通过溶胶-凝胶过程形成在MAO处理表面上的平均尺寸为200nm的纳米颗粒及其水接触角。
图3(a)和(b)示出了通过EDX在MAO处理样品上的Ni沉积表面的SEM图以及表面上的Ni分布。
图4(a)和(b)示出了通过EDX在MAO处理样品上的Ni沉积横截面的SEM图以及横截面的Ni分布。
图5(a)和(b)示出了通过溶胶-凝胶处理的MAO处理样品的黑色着色。在处理过程中使用不同的硅烷。两个样品的颜色基本上是相同的并且与标准颜色代码PANTONE 19-0303相匹配。
图5(c)示出了在退火之前和之后通过溶胶-凝胶过程进一步处理的MAO样品的XRD峰值。
图5(d)示出了在退火之前和之后通过溶胶-凝胶过程进一步处理的MAO样品的拉曼位移。
具体实施方式
如此处和权利要求书中，“包括”表示包含下列元件，但是并不排除其他。
如此处和权利要求书中，除非另有说明，“联接”或者“连接”指的是直接或者通过一个或者多个电子装置间接电联接或者连接。
如此处和权利要求书中，“MAO处理的镁合金”指的是镁合金，该镁合金包括在MAO处理期间形成在镁合金表面上的镁基陶瓷层。
本发明涉及在微弧氧化(MAO)处理的镁合金的表面上形成功能性涂层、以及通过疏水性处理改变其耐腐蚀性、通过化学镀镍沉积改变电气性质和通过溶胶-凝胶过程而增强颜色外观的方法。
实施例1，MAO处理
由商品等级镁合金AZ31B制成的样品在实验中使用，并且其化学成分列在了表格1中。本领域技术人员将知晓包括至少88％Mg的其他Mg合金也适于本发明。具有30mm x 30mmx 1mm尺寸的样品通过微弧氧化方法进行了处理。首先，用于MAO处理的电解液是通过将20-30g/L硅酸盐、5-30g/L磷酸盐和3-6g/L氢氧化物溶解到不锈钢容器内的DI水中而制备的。然后，电流强度33-89A/dm2的电流施加到已浸入到电解液容器中的镁合金样品上，以脉冲频率500-2600Hz持续240-720秒。化学和机械保护的镁基陶瓷层是在处理期间形成在其表面上。其水接触角是91.4°。该表面是电绝缘的。
表格1，镁合金AZ31B的化学成分
| 成分 | Al | Zn | Mn | Mg |
| 重量[％] | 3.17 | 0.78 | 0.31 | 平衡 |
实施例2，疏水性处理
在本发明的一个实施方式中，提供了在MAO处理的镁合金(MAO样品)上的疏水性处理过程。化学蚀刻过程是通过在室温下将MAO样品浸入到0.125mol/L NaOH溶液持续24小时而进行的。具有100-200nm长度的精细的纳米结构，如图1(a)和(b)中示出那样，形成在MAO处理表面上。鳞片状结构形成在微孔MAO处理的镁合金的表面上，这将促进改善的疏水性。然后，所蚀刻的样品已经在室温下浸入到包含1g全氟癸基三甲氧基硅烷(或者0.4g正辛基三乙氧基硅烷或1g全氟癸基硅烷)以及10g乙醇的溶液中持续1小时，以形成非常薄的硅烷层，随后在180℃下进行干燥处理1小时。其水接触角增加到145.8°。
在本发明的另一实施方式中，提供了第二疏水性处理方法。四乙基原硅酸酯(TEOS)和乙醇(5mL)以滴液的方式缓慢地增加到NH4OH、H2O和C2H5OH(30.5mL)的混合物中。该混合物可在60℃下搅拌75分钟，以获得硅胶体。溶胶溶液从透明变换到白色不透明。MTES(1.6mL)和乙醇(5mL)然后以滴液方式缓慢增加到混合溶液中。该溶液在60℃下搅拌19小时，并且在环境温度下进一步沉降3天。可以获得白色不透明溶液。MAO样品被浸入到疏水性硅溶胶-凝胶中持续15分钟，并且缓慢抽出，并且在110℃下干燥30分钟，以移除剩余的溶剂。该程序重复两次，以将附加的膜形成在MAO处理表面上。该膜及其水接触角分别在图2(a)和(b)中示出。其水接触角被增加到140.4°。
MAO样品的耐腐蚀性由于增强的疏水性而同样得到改善。具体地说，对于上述的第二疏水性处理，随着在MAO表面的顶部上存在纳米颗粒附加层，盐雾试验进行的操作比没有进行疏水处理更好，如在盐雾试验期间通过第二疏水性处理的表面上没有黑点。
实施例3，导电处理
下列三个步骤化学镀镍沉积程序旨在将导电涂层形成在MAO处理的镁合金(MAO样品)上。第一个步骤是预处理过程，其中MAO样品浸入到醋酸镍的2g/L乙醇溶液中，在室温下持续20s，并且通过DI水进行冲洗。
第二步骤是活化过程，其中MAO样品被浸入到NaBH4的8g/L乙醇溶液中，在室温下持续5分钟，并且通过DI水进行冲洗。NaBH4用作还原剂，来将醋酸镍中的镍离子还原成活化的镍原子，从而一些被还原的镍颗粒形成在MAO处理表面的气孔中；在这种情况下，这些被还原的镍颗粒作为镍层生长的起始。
第三个步骤是化学镀镍沉积过程，其中混合水溶液是由NiSO4·6H2O：10-50g/L、NaH2PO2·H2O：20-40g/L、柠檬酸钠：20g/L、H3BO3(硼酸)：20g/L、C3H6O3(乳酸)：15mL/L、硫脲：0-2mg/L所形成。MAO样品浸入到混合水溶液(pH 10-11)中，在70℃下持续50分钟，并且通过DI水进行冲洗。图3(a)和(b)示出了通过EDX的MAO样品上NI沉积表面的SEM图以及表面上的Ni分布。图4(a)和(b)示出了通过EDX的MAO样品上Ni沉积的横截面的SEM图以及横截面的Ni分布。镍以10μm厚度沉积在MAO处理表面的顶部上。其表面电阻通过四点探针方法进行测量是≤0.05Ω/sq。这个结果表示了具有较高均匀性和耐腐蚀性的镍层通过化学镀镍被沉积在MAO处理表面上。
根据EDX结果，示出了镍均匀沉积在MAO处理表面上。这些表面的新组合可用于电子壳体材料，尤其是用于需要优秀耐腐蚀性和导电性，例如户外照明固定装置和户外便携电子设备等等。
实施例4，颜色处理
为了MAO处理表面上的颜色处理，溶液通过混合TEOS(1-10g)和C2H5OH(20-100mL)、NH4OH(1-10mL)以及水(0-5mL)所形成。该混合物在60℃下搅拌60分钟。三乙氧基(辛基)硅烷(OTES)(1-10mL)被以滴的形式增加到混合溶液中。该混合物在60℃下连续搅拌6小时，然后在室温下陈化24小时。MAO样品被浸入到疏水性硅溶胶中，持续10分钟，然后在100℃下干燥30分钟，以移除剩余的溶剂。该程序重复三次以上，以获得足够厚的硅膜。在浸涂层之后，样品在真空下在400℃下退火2小时。然后黑色着色形成在MAO处理表面上，以满足市场的美学需要。
图5(a)和(b)示出了通过溶胶-凝胶过程进行MAO处理样品的均匀黑色着色。两个样品的着色基本上是相同的，并且与标准颜色代码PANTONE 19-0303相匹配。图5(c)示出了处理表面的XRD，其中蓝色曲线表示在着色之前的MAO样品，而红色曲线表示了着色之后的MAO样品表面。黑色被认为是在退火期间产生的石墨。在图5(d)中，处理表面的拉曼谱被示出，其中，红色曲线表示着色之前的MAO样品，而黑色曲线表示着色之后的MAO样品。在1350cm-1处黑色曲线的典型峰值表示了退火之后的石墨存在。
本发明的示范性实施方式进行了描述。尽管该描述是参照特定的实施方式，但是对于本领域技术人员而言清楚本发明可通过这些特定细节的变形而实现。因此，本发明将并不限于在此说明的实施方式。
参考文献：
1J.E.Gray,B.Luan的“镁及其合金上的保护涂层--关键评论”，Journal ofAlloys and Compounds 336(2002)，第88-113页。
Claims (10)
1.一种微弧氧化处理的镁合金表面的处理方法，其包括：
提供微弧氧化处理的镁合金样品；
将所述镁合金样品浸入到醋酸镍的2g/L的乙醇溶液中作预处理；
将经过预处理的所述镁合金样品浸入到还原剂溶液中作活化处理，以将被还原的镍颗粒形成在微弧氧化处理表面的气孔中；
将经过活化处理的所述镁合金样品沉积在混合水溶液中，在已活化的所述镁合金样品的表面上形成化学镀镍；
其中，在所述表面上形成化学镀镍的镁合金样品是导电的。
2.如权利要求1所述的方法，其中所述还原剂溶液是NaBH4的8g/L乙醇溶液。
3.如权利要求1所述的方法，其中所述混合水溶液包括NiSO4·6H2O、NaH2PO2·H2O、柠檬酸钠、H3BO3、C3H6O3以及硫脲。
4.如权利要求3所述的方法，其中所述混合水溶液包括：
10–50g/L NiSO4·6H2O；
20–40g/L NaH2PO2·H2O；
20g/L柠檬酸钠；
20g/L H3BO3；
15mL/L C3H6O3；以及
0–2mg/L硫脲。
5.如权利要求1所述的方法，其中所述在表面上形成化学镀镍的镁合金样品的表面电阻为小于等于0.05Ω/sq。
6.如权利要求1所述的方法，其中所述预处理是在室温下进行20s。
7.如权利要求1所述的方法，其中所述活化处理是在室温下进行5分钟。
8.一种镁合金，其包括：
所述镁合金上具有5-40μm厚度的微弧氧化处理的层；和
在微弧氧化处理的层上具有10-30μm厚度的镍层；
其中，所述镍层形成了所述微弧氧化处理层上的均匀表面，从而所述合金具有小于等于0.05Ω/sq的表面电阻。
9.如权利要求8所述的镁合金，其中所述微弧氧化处理层具有孔，该孔具有由镍填充的1-3μm的平均孔径。
10.如权利要求8所述的镁合金，其通过如权利要求1所述的方法制造。
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| US14/543,911 US20150140314A1 (en) | 2013-11-21 | 2014-11-18 | Surface treatment method on Micro-arc Oxidation treated Mg alloys |
| CN201410666132.8A CN104862699A (zh) | 2013-11-21 | 2014-11-19 | 微弧氧化处理的镁合金上的表面处理方法 |
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Cited By (1)
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|---|---|---|---|---|
| CN110714219A (zh) * | 2019-11-04 | 2020-01-21 | 吉林大学 | 镁合金微弧氧化表面电镀镍的方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119845A (zh) * | 2016-06-25 | 2016-11-16 | 袁春华 | 一种耐摩擦抗腐蚀镁合金的制备方法 |
| CN106222647A (zh) * | 2016-07-23 | 2016-12-14 | 中信戴卡股份有限公司 | 一种镁合金表面处理方法 |
| EP3391915B1 (en) | 2017-03-30 | 2021-04-14 | Biomet Manufacturing, LLC | Methods of modifying the porous surface of implants |
| CN109183126A (zh) * | 2018-08-11 | 2019-01-11 | 桂林理工大学 | 一种镁合金表面疏水膜层的制备方法 |
| CN109055841B (zh) * | 2018-09-06 | 2020-08-25 | 中国石油大学(华东) | 铸造可溶镁合金复合材料压裂球表面防护层制备方法 |
| CN113046811B (zh) * | 2019-12-27 | 2022-12-09 | 比亚迪股份有限公司 | 一种微弧氧化电解液及其应用方法、工件 |
| CN111394771B (zh) * | 2020-04-22 | 2021-05-04 | 哈尔滨工业大学 | 一种在铜及其合金表面制备涂层的方法及铜制品 |
| CN111893542B (zh) * | 2020-08-06 | 2021-08-03 | 牡丹江申佳合金材料有限公司 | 一种超疏水型微弧氧化耐磨涂层的钛合金及其制法 |
| CN113373492B (zh) * | 2021-04-30 | 2022-08-16 | 上海交通大学 | 一种镁合金超高频微弧氧化的处理方法 |
| CN113668035B (zh) * | 2021-07-15 | 2024-02-06 | 桂林理工大学 | 一种于微弧氧化镁合金表面一步原位生成Zn-MOF涂层及其制备方法 |
| CN113604851B (zh) * | 2021-07-15 | 2024-02-06 | 桂林理工大学 | 一种镁合金表面无需低表面能物质修饰的超疏水涂层及其制备方法 |
| CN114672864A (zh) * | 2022-04-25 | 2022-06-28 | 齐鲁工业大学 | 一种医用镁合金微弧氧化复合涂层的制备方法 |
| CN114606550B (zh) * | 2022-04-25 | 2023-04-11 | 齐鲁工业大学 | 生物医用镁合金制品的电解液及表层制备方法 |
| CN114941164B (zh) * | 2022-06-16 | 2024-01-19 | 河南大学 | 一种镁合金表面双功能复合涂层的制备方法 |
| CN115418641A (zh) * | 2022-09-08 | 2022-12-02 | 南通大学 | 一种金属材料超疏水防腐表面的制备方法 |
| CN115613103B (zh) * | 2022-11-07 | 2023-07-11 | 南京工程学院 | 微弧氧化镁合金表面疏水Mg-Al类水滑石膜及其一步制备方法和应用 |
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- 2014-11-19 CN CN201710598780.8A patent/CN107523814A/zh active Pending
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| US20170137945A1 (en) | 2017-05-18 |
| US20150140314A1 (en) | 2015-05-21 |
| CN104862699A (zh) | 2015-08-26 |
| HK1208506A1 (zh) | 2016-03-04 |
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