CN111020574A - Low-temperature preparation method of hydrophobic heat exchange material based on stainless steel and graphene - Google Patents
Low-temperature preparation method of hydrophobic heat exchange material based on stainless steel and graphene Download PDFInfo
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- CN111020574A CN111020574A CN201911252818.1A CN201911252818A CN111020574A CN 111020574 A CN111020574 A CN 111020574A CN 201911252818 A CN201911252818 A CN 201911252818A CN 111020574 A CN111020574 A CN 111020574A
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 117
- 239000010935 stainless steel Substances 0.000 title claims abstract description 117
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 34
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000010949 copper Substances 0.000 claims abstract description 28
- 229910052802 copper Inorganic materials 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims description 28
- 238000009713 electroplating Methods 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 14
- 238000007747 plating Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 239000010410 layer Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 150000001879 copper Chemical class 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004327 boric acid Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 150000002431 hydrogen Chemical class 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
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 238000000861 blow drying Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical class CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 2
- 150000001299 aldehydes Chemical class 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 150000001345 alkine derivatives Chemical class 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000002152 aqueous-organic solution Substances 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 230000005484 gravity Effects 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- 229940077386 sodium benzenesulfonate Drugs 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims 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 claims description 2
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 238000007772 electroless plating Methods 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 description 12
- 230000005494 condensation Effects 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 238000000576 coating method Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 229910000365 copper sulfate Inorganic materials 0.000 description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—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
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- 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
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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
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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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
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a low-temperature preparation method of a hydrophobic heat exchange material based on stainless steel and graphene, wherein the stainless steel is adopted as a substrate material, copper or nickel is plated on the surface of the stainless steel, and then graphene is deposited on the surface of the stainless steel under the low-temperature condition (500-900 ℃) by a plasma enhanced chemical vapor deposition method, so that the influence of the deposition temperature of the graphene on the mechanical property of the stainless steel can be greatly reduced, and in addition, only one metal is plated on the surface of the stainless steel in the pretreatment process, so that the operation is simpler.
Description
Technical Field
The invention relates to stainless steel and graphene, in particular to a preparation method of a hydrophobic heat exchange material based on stainless steel and graphene.
Background
Stainless steel is widely used in important fields such as heat exchange, water industry, gas transmission and the like, more than 50% of condenser pipes of a thermal power plant adopt stainless steel pipes at present, and more parts gradually adopt the stainless steel pipes in the field of seawater desalination in recent years.
In the use process of the condensation pipe, if the condensation wall has strong hydrophilicity, a liquid film is formed on the surface of the condensation wall after steam is condensed and is attached to the surface of the condensation wall, and the thickness of the liquid film layer determines the quality of the film-shaped condensation heat transfer performance. If the condensation wall has strong hydrophobicity, the condensation liquid is not easy to spread on the wall surface to form a film, but forms a plurality of drops with random distribution and different sizes, and the condensation is in a drop-shaped condensation form. In this case, the latent heat of vaporization released by condensation can be directly transferred to the wall surface, and therefore, the heat transfer coefficient of the droplet-like condensation is several times to ten times that of the corresponding film-like condensation under the same conditions.
With the wide application of graphene in this year, researchers find that depositing a layer of graphene on the surface of a stainless steel tube can significantly improve the hydrophobicity of the stainless steel, because the graphene itself has excellent stability, corrosion resistance and hydrophobicity. Therefore, several technical approaches to deposit graphene onto stainless steel surfaces have been followed.
For example, a method of depositing graphene on the surface of a copper pipe, which is to prepare graphene paste mainly by using organic binders such as epoxy resin and the like, and then coating the graphene paste on the surface of a stainless steel pipe. For example, chinese patent publication No. CN106871705A, published as 6 and 20 in 2017, discloses a technical solution for depositing a graphene/epoxy resin coating on the surface of a copper pipe for corrosion protection, but this method greatly affects the size and finish of the pipe body and is prone to shedding. For another example, patent document CN106802106A discloses a method for preventing corrosion by depositing graphene on the surface of a copper tube by chemical vapor deposition, wherein the copper tube is used as the substrate. For another example, the chinese patent publication No. CN107034498A, published as 8/11/2017, discloses a technical scheme of electroplating copper after electroplating nickel on the surface of stainless steel, and then depositing graphene on the surface of the stainless steel by chemical vapor deposition, so as to be used for corrosion prevention of stainless steel of an industrial grounding grid.
Disclosure of Invention
In order to solve various technical defects in the prior art, the invention provides a preparation method of a hydrophobic heat exchange material based on stainless steel and graphene, the method can use industrial-grade stainless steel as a substrate material, copper or nickel is plated on the surface of the industrial-grade stainless steel, then graphene is deposited on the surface of the stainless steel by a Plasma Enhanced Chemical Vapor Deposition (PECVD) method under a low-temperature condition, the influence of the deposition temperature of the graphene on the mechanical property of the stainless steel can be greatly reduced, and the method only plates one metal on the surface of the stainless steel in a pretreatment process, so that the operation is simpler.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a hydrophobic heat exchange material based on stainless steel and graphene comprises the following steps:
plating copper or nickel on the surface of stainless steel by chemical plating or electroplating; the stainless steel is 304 or 316, and the stainless steel can be stainless steel sheet, stainless steel tube, stainless steel powder, stainless steel block or other shapes.
And (II) putting the stainless steel subjected to nickel or copper plating into a chemical vapor deposition reaction chamber, reducing the pressure of the reaction chamber to be less than 5 Pa, introducing hydrogen, simultaneously starting to heat up, keeping the temperature for 1 min-60 min after the temperature is raised to 500-900 ℃, introducing carbon-containing gas, simultaneously opening plasma equipment to ionize the gas, keeping the temperature for 1 min-60 min to crack the carbon-containing gas and deposit the carbon-containing gas on the surface of the stainless steel to form graphene, then cooling, and completing the chemical vapor deposition of the graphene on the stainless steel to obtain the hydrophobic heat exchange material based on the stainless steel and the graphene.
When the chemical plating method is adopted in the step (one): cleaning the surface of the stainless steel by using acetone or absolute ethyl alcohol and drying the stainless steel by blowing, and then cleaning the surface of the stainless steel by using deionized water and drying the stainless steel by blowing; chemical impurity removal is carried out by dilute hydrochloric acid, and then the product is cleaned by deionized water and dried; cleaning the surface of the glass substrate with acetone or absolute ethyl alcohol again and drying the glass substrate; and (3) placing the washed stainless steel in a nickel or copper salt solution, standing for a period of time to form a precursor on the surface of the stainless steel, taking out the precursor, drying, and then placing the dried precursor into a reducing agent solution for reduction to obtain the nickel or copper plated stainless steel.
During blow-drying, the used gas is inert gas, including nitrogen and argon.
The cleaning process comprises a washing process and an ultrasonic vibration cleaning process.
When chemical impurity removal is carried out, the concentration of the used dilute hydrochloric acid is 0.1-2 mol/L, and the chemical impurity removal time is 1-30 min.
The nickel or copper salt solution is one or more aqueous solutions or organic solutions of nickel or copper sulfate, carbonate, nitrate, oxalate, acetate, chloride and acetylacetone salt in any proportion, and the specific gravity of the nickel or copper in the solution is 0.1-5 wt%; meanwhile, the additive of the nickel or copper salt solution is one or more of methanol, ethanol, sodium dodecyl benzene sulfonate and dimethylformamide mixed solution in any proportion; the reducing agent solution is one or a mixture of more of potassium borohydride, sodium borohydride, glucose, hydrazine hydrate and ammonia water in any proportion; the additive in the reducing agent solution is one or a mixture of more of sodium citrate, sodium acetate, sodium benzenesulfonate, thiourea and glycol in any proportion.
When the electroplating method is adopted in the step (one): stainless steel is connected with the negative electrode of a constant current power supply, nickel or copper is connected with the positive electrode of the constant current power supply, and the positive electrode and the negative electrode are placed in electroplating liquid containing nickel or copper to be electroplated for 0.5min to 10min under the voltage of 1V to 10V.
The components of the electroplating solution comprise: 10g/L to 100g/L of nickel sulfate, 10g/L to 300g/L of nickel chloride, 10g/L to 100g/L of boric acid and 0.1g/L to 10g/L of sodium dodecyl sulfate.
In the step (II):
the chemical vapor deposition reaction chamber uses a quartz tube, and both ends of the quartz tube are sealed and sealed by a flange and a rubber ring; and (4) reducing the pressure by adopting a mechanical pump, and connecting the quartz tube with the mechanical pump.
The power control range of the used plasma equipment is 10W-100W.
The protective gas is argon.
The introduced hydrogen is pure hydrogen, and the hydrogen and argon account for the following ratio: 0.1-5%, the flow rate of the introduced hydrogen is 0.5-500 sccm, and the temperature rise rate after the introduction of the hydrogen is 5-15 ℃/min.
The carbon-containing gas is one or more of alkane, alkene, alkyne, aromatic hydrocarbon, alcohol, aldehyde and ketone with carbon atoms within the range of 1-10 in any proportion; the carbon-containing gas and the protective gas are 0.1-5% in proportion, the flow of the introduced carbon-containing gas is 0.5-500 sccm, and the protective gas is argon.
The hydrophobic heat exchange material based on stainless steel and graphene prepared by the method can be deposited to obtain a graphene film comprising a single layer or multiple layers.
Compared with the prior art, the invention has the following beneficial effects:
1. the deposition of graphene can be completed at 500-900 ℃ by the plasma enhancement device, and the number and quality of graphene layers can be regulated and controlled by adjusting the power of the plasma enhancement device.
2. The stainless steel nickel or copper plating adopts a chemical plating or electroplating method, and only one metal is plated.
3. The method for depositing the graphene has the advantages of simple operation process, less equipment requirement and low manufacturing cost.
4. The thickness of the plated metal layer is only dozens of nanometers, and the generated additional heat resistance is very small, so that the size and the use of the stainless steel are not influenced.
5. The hydrophobic coating of the stainless steel has excellent hydrophobic property, and can greatly improve the hydrophobic property of the stainless steel.
Drawings
FIG. 1 is a graph showing surface Raman spectrum data of the hydrophobic heat exchange material prepared in example 1.
FIG. 2 is a graph showing contact angle test data of the hydrophobic heat exchange material prepared in example 1.
Wherein 1 is a contact angle of stainless steel on which graphene is not deposited, and 2 is a contact angle of stainless steel on which graphene is deposited.
Detailed Description
The present invention will be further described with reference to specific examples to better understand the contents of the present invention, but the present invention is not limited to the following examples.
Example 1
A preparation method of a hydrophobic heat exchange material based on stainless steel and graphene comprises the following steps:
plating copper or nickel on the surface of stainless steel
The stainless steel is 304 or 316, and the stainless steel can be stainless steel sheet, stainless steel tube, stainless steel powder, stainless steel block or other shapes.
Wherein, chemical nickel plating is adopted: chemical impurity removal is carried out on stainless steel by using dilute hydrochloric acid, then cleaning and blow-drying are carried out, the stainless steel is placed in 2wt% of nickel sulfate and 0.2wt% of sodium dodecyl benzene sulfonate aqueous solution, the stainless steel is taken out and dried after standing for 15min, the stainless steel is placed in 0.1wt% of sodium borohydride aqueous solution, the stainless steel is taken out after reaction for 15min, and surface chemical nickel plating is finished. The acid solution is hydrochloric acid, the concentration is 5 mol/L, and the chemical impurity removal time is 15 min; the liquids used for cleaning were acetone and water. The concentration of the used dilute hydrochloric acid is 1 mol/L, and the chemical impurity removal time is 15 min.
(II) preparing graphene hydrophobic coating
Putting the stainless steel after nickel or copper plating into a chemical vapor deposition reaction chamber, sealing, introducing hydrogen with the gas flow of 500sccm, reducing the pressure of the reaction chamber to 0.5 Pa, heating from room temperature to 500 ℃, keeping the temperature rise rate at 5 ℃/min, and keeping the temperature at 500 ℃ for 60 min; and then simultaneously introducing methane with the flow rate of 500sccm, simultaneously opening a plasma device to ionize gas, controlling the plasma power to be 100W, then preserving the temperature for 60min to crack the carbon-containing gas and deposit the carbon-containing gas on the surface of the stainless steel to form graphene, and then cooling to obtain the hydrophobic heat exchange material based on the stainless steel and the graphene.
As shown in fig. 1, a raman test data graph of the hydrophobic heat exchange material prepared in this experimental example shows that there is an obvious characteristic peak of graphene, which indicates that the preparation of the graphene hydrophobic coating on the stainless steel is successfully achieved in this example.
Example 2
This example used substantially the same procedure as example 1, except that: heating from room temperature to 900 deg.C, and maintaining at 900 deg.C during deposition.
Example 3
This example used substantially the same procedure as example 1, except that: the flow rate of methane was 250 sccm.
Example 4
This example used substantially the same procedure as example 1, except that: the flow rate of methane was 0.5 sccm.
Example 5
This example used substantially the same procedure as example 1, except that: the flow rate of hydrogen was 250 sccm.
Example 6
This example used substantially the same procedure as example 1, except that: the flow rate of hydrogen was 0.5 sccm.
Example 7
This example used substantially the same procedure as example 1, except that: the stainless steel is one or more of a stainless steel pipe, a stainless steel film and a stainless steel block.
Example 8
This example used substantially the same procedure as example 1, except that: in the pretreatment step of the stainless steel, the stainless steel is subjected to electro-polishing treatment after chemical impurity removal by using dilute hydrochloric acid, and the polishing solution comprises phosphoric acid: ethylene glycol: the volume ratio of acetic acid is 1:1:1, and the polishing voltage is 1V.
Example 9
This example used substantially the same procedure as example 1, except that: the heating rate was 15 ℃/min.
Example 10
This example used substantially the same procedure as example 1, except that: heating from room temperature to 500 deg.C, heating at a rate of 5 deg.C/min, and maintaining at 500 deg.C for 1 min.
Example 11
This example used substantially the same procedure as example 1, except that: and introducing methane with the flow of 500sccm, simultaneously opening a plasma device to ionize gas, controlling the plasma power to be 100W, and then preserving heat for 1 min.
Example 12
This example used substantially the same procedure as example 1, except that: copper is chemically plated on the surface of the stainless steel, and the copper solution is 2wt% of copper sulfate and 0.2wt% of sodium dodecyl benzene sulfonate aqueous solution.
Example 13
This example used substantially the same procedure as example 1, except that: the surface of the stainless steel is electroplated with nickel, and the electroplating steps are as follows: connecting stainless steel with the negative electrode of a constant current power supply, connecting nickel or copper with the positive electrode of the constant current power supply, placing the two electrodes in nickel-containing electroplating solution, and electroplating for 10min under the voltage of 10V, wherein the electroplating solution is as follows: 100g/L of nickel sulfate, 300g/L of nickel chloride, 100g/L of boric acid and 10g/L of sodium dodecyl sulfate.
Example 14
This example used substantially the same procedure as example 1, except that: electroplating copper on the surface of stainless steel, wherein the electroplating step is as follows: connecting stainless steel with the negative pole of a constant current power supply, connecting nickel or copper with the positive pole of the constant current power supply, placing the two poles in copper-containing electroplating solution, and electroplating for 10min under the voltage of 10V, wherein the electroplating solution is as follows: 100g/L copper sulfate, 300g/L copper chloride, 100g/L boric acid and 10g/L sodium dodecyl sulfate.
Example 15
This example used substantially the same procedure as example 1, except that: the power of the plasma was controlled at 10W.
Hydrophobic layers and other extended hydrophobic coatings can also be deposited on the stainless steel surface by this method.
Claims (14)
1. A low-temperature preparation method of a hydrophobic heat exchange material based on stainless steel and graphene is characterized by comprising the following steps: plating copper or nickel on the surface of stainless steel by chemical plating or electroplating; and (II) putting the stainless steel subjected to nickel or copper plating into a chemical vapor deposition reaction chamber, reducing the pressure of the reaction chamber to be less than 5 Pa, introducing hydrogen, simultaneously starting to heat up, keeping the temperature for 1 min-60 min after the temperature is raised to 500-900 ℃, introducing carbon-containing gas, simultaneously opening protective gas of plasma equipment, keeping the temperature for 1 min-60 min to crack the carbon-containing gas and deposit the carbon-containing gas on the surface of the stainless steel to form graphene, then cooling, and finishing the chemical vapor deposition of the graphene on the stainless steel to obtain the hydrophobic heat exchange material based on the stainless steel and the graphene.
2. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 1, wherein the electroless plating is specifically performed by: cleaning the surface of the stainless steel, chemically removing impurities, and drying; and then placing the stainless steel in a nickel or copper salt solution, standing until a precursor is formed on the surface of the stainless steel, taking out and drying the stainless steel, and then placing the stainless steel with the precursor into a reducing agent solution for reduction to obtain the nickel or copper plated stainless steel.
3. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 2, wherein the operations of cleaning, chemical impurity removal and blow-drying are as follows: cleaning the surface of the stainless steel by using acetone or absolute ethyl alcohol and drying the stainless steel by blowing, and cleaning the surface of the stainless steel by using deionized water and drying the stainless steel by blowing; then dilute hydrochloric acid is used for chemical impurity removal, and then deionized water is used for cleaning the surface of the stainless steel and drying the stainless steel; and cleaning the surface of the stainless steel by using acetone or absolute ethyl alcohol and drying.
4. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 3, characterized in that: the concentration of the dilute hydrochloric acid is 0.1-2 mol/L, and the chemical impurity removal time is 1-30 min; the liquid used for cleaning is a mixed liquid of acetone, alcohol, isopropanol and water.
5. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 2, characterized in that: the nickel or copper salt solution is one or more aqueous solutions or organic solutions of sulfate, carbonate, nitrate, oxalate, acetate, chloride and acetylacetone salt in any proportion, wherein the specific gravity of nickel or copper in the solution is 0.1-5 wt%.
6. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 2, characterized in that: the reducing agent solution is one or more of potassium borohydride, sodium borohydride, glucose, hydrazine hydrate and ammonia water in any proportion; the additive in the reducing agent solution is one or a mixed liquid of sodium citrate, sodium acetate, sodium benzenesulfonate, thiourea and glycol in any proportion.
7. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 1, wherein the electroplating is specifically performed by: connecting stainless steel with the negative electrode of a constant current power supply, connecting nickel or copper with the positive electrode of the constant current power supply, placing the positive electrode and the negative electrode in electroplating liquid containing nickel or copper, and electroplating for 0.5-10 min under the voltage of 1-10V.
8. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 1, characterized in that: the components of the electroplating solution comprise: 10g/L to 100g/L of nickel sulfate, 10g/L to 300g/L of nickel chloride, 10g/L to 100g/L of boric acid and 0.1g/L to 10g/L of sodium dodecyl sulfate.
9. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 1, characterized in that: the power of the plasma equipment is 10W-100W.
10. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 1, characterized in that: the introduced hydrogen is pure hydrogen, and the proportion of the hydrogen to the protective gas is as follows: 0.1-5%, the flow rate of the introduced hydrogen is 0.5-500 sccm, and the protective gas is argon.
11. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 1, characterized in that: the temperature rise rate after the hydrogen is introduced is 5-15 ℃/min.
12. The low-temperature preparation method of the stainless steel and graphene-based hydrophobic heat exchange material according to claim 1, characterized in that: the carbon-containing gas is one or more of alkane, alkene, alkyne, aromatic hydrocarbon, alcohol, aldehyde and ketone with carbon atoms within the range of 1-10 in any proportion; the carbon-containing gas and the protective gas are 0.1-5% in proportion, the flow of the introduced carbon-containing gas is 0.5-500 sccm, and the protective gas is argon.
13. The low-temperature preparation method of the hydrophobic heat exchange material based on the stainless steel and the graphene, according to claim 1, wherein the prepared graphene film deposited on the hydrophobic heat exchange material based on the stainless steel and the graphene comprises a single layer or 2-10 layers.
14. The method of claim 1, wherein: the stainless steel is 304 or 316, and the stainless steel is in the shape of a sheet, a tube, a block or powder.
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