CN103774125B - A kind of heat treatment method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer - Google Patents
A kind of heat treatment method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer Download PDFInfo
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- CN103774125B CN103774125B CN201410046721.6A CN201410046721A CN103774125B CN 103774125 B CN103774125 B CN 103774125B CN 201410046721 A CN201410046721 A CN 201410046721A CN 103774125 B CN103774125 B CN 103774125B
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 50
- 238000010438 heat treatment Methods 0.000 title claims abstract description 42
- 238000007747 plating Methods 0.000 title claims abstract description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910001096 P alloy Inorganic materials 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 16
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 30
- 238000000576 coating method Methods 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000003223 protective agent Substances 0.000 claims abstract description 18
- 239000011574 phosphorus Substances 0.000 claims abstract description 15
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 14
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 9
- LWHQXUODFPPQTL-UHFFFAOYSA-M sodium;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoate Chemical compound [Na+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F LWHQXUODFPPQTL-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 claims description 15
- 239000000126 substance Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 7
- 229910018104 Ni-P Inorganic materials 0.000 description 5
- 229910018536 Ni—P Inorganic materials 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000010183 spectrum analysis Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- QDWJUBJKEHXSMT-UHFFFAOYSA-N boranylidynenickel Chemical compound [Ni]#B QDWJUBJKEHXSMT-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- -1 boron amide alkane Chemical class 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011814 protection agent Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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Abstract
The invention discloses a kind of heat treatment method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer. First the present invention is placed in thermostatic drying chamber by aluminum alloy part, is heated to 200 DEG C, and then constant temperature 30min takes out, cooling in air; Secondly in boric acid spirit solution, add Sodium perfluorooctanoate as activating agent, after stirring, form heat treatment protective agent, the aluminum alloy part after drying is put into protective agent, soak 5-10min, soaking temperature is 20 DEG C-40 DEG C; Finally by soaking aluminum alloy part after heat treatment protective agent, to put into temperature be the Muffle furnace of 380 DEG C-450 DEG C, and constant temperature 40-60min heat treatment, then takes out, and air is cooling. The present invention, by protective agent pretreatment, can ensure that amorphous state chemistry nickel plating phosphorus coating is after antivacuum heat treatment, Hv >=850, and ensure that coating color does not change.
Description
Technical field
The present invention relates to a kind of heat treatment method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer.
Background technology
Aluminium alloy has the features such as mechanical strength is high, density is little, heat-conductivity conducting is good, good toughness, easy processing,Thereby in industry, be a most widely used class non-ferrous metal structural material, especially at Aero-Space, vapourIn car, machine-building, boats and ships and chemical industry, widely apply. Aluminum alloy surface covers the oxidation of one deck densificationFilm, it can be kept apart aluminium alloy and surrounding environment, avoids oxidized. But this layer of oxide-film is vulnerable toThe corrosion of strong acid and highly basic, aluminium alloy easily produces intercrystalline corrosion simultaneously, and case hardness is low, not wear-resisting.
Along with the development of industrial technology, the continuous expansion of application, service condition complicated, rightPart prepared by aluminium alloy, as propositions such as high-end automobile brake spool, refitting equipment connector, cabinet guide railsCase hardness and the wearability requirement of more and more doing. Therefore to carry out wearability and raising to aluminum alloy surfaceHardness processing. Use at present more technique to have: durionise, differential arc oxidation, chemical plating nickel-phosphorus alloy,Chemical nickel plating ni-b alloy. Aluminium alloy surface electric plating chromium (although 15 μ m) have a high rigidity (850-1100Hv),But owing to having very large environmental pollution, hexavalent chromium is strong carcinogen, and country does not advocate, alsoDo not there is sustainable developability. Carry out differential arc oxidation in aluminum alloy surface, can obtain hardness and be 450Hv andThe inside/outside duplicature of 1600Hv, but differential arc oxidation is only suitable for the parts of simple shape, and power consumption is large. ChemistryNickel plating has the following advantages: without energising, comparatively environmental protection; Thickness of coating and even, processing unit is not subject toShape restriction, indeformable, be particularly applicable to complex-shaped, high tiny and large of dark blind hole and required precisionThe surface treatment of type parts; There is good anti-corrosion resisting property, in much acid, alkali, salt, ammonia and seawaterHave good corrosion resistance, its corrosion resistance is than superior many of stainless steel; Parts after treatment, any surface finishSpend highly, surface-brightening, does not need machining and polishing again, the use of can directly installing; Coating and baseThe adhesion of body is high, incrust, and its adhesion is higher than durionise and ion plating. So chemical nickel platingIt is the prefered method that improves aluminum alloy surface wearability and hardness. At present, conventional mainly contain chemical Ni-P andTwo kinds of techniques of chemical nickel boron. Wherein chemical Ni-P can be divided into again low-phosphorous (phosphorous 2-5% according to the difference of phosphorus contentMass percent), middle phosphorus (phosphorous 6-9% mass percent), high phosphorus (phosphorous 10-14% mass percent).Under three kinds of composition plated states, coating is amorphous Ni-P alloy, plated state hardness be respectively 650-800Hv,500-650Hv, 350-500Hv, the service condition (Hv >=850) that meet high abrasion, high rigidity also will be enteredRow heat treatment, but hardness low-phosphorous and middle phosphorus chemistry nickel-phosphorus coating does not rise counter falling after heat treatment, only hasIt is to make hardness improve that high-phosphorus chemical nickel phosphorus coating is heat-treated above at 300 DEG C, various experimental result tablesBright, optimum treatment process is 400 DEG C of heat treatment 1h, and the coating hardness obtaining can reach 900-1100Hv.(above-mentioned various nickel-phosphorus coating thickness is 15 μ m, and coating hardness adopts HX1000 microhardness instrumentationExamination, test condition is: 50g, 15s. ) this is that Amorphous Ni-P Alloy layer starts crystallization, diffusion-precipitation at 350 DEG CNi3P phase, improves coating hardness greatly, and reaches best at 400 DEG C/1h because raise along with temperature orPerson's time lengthening, crystalline state Ni3P constantly grows up mutually, can make on the contrary coating hardness reduce. Chemical nickel boron obtainsAlloy layer (15 μ m) can reach 750-850Hv under plated state state, substantially can meet wearability, butBecause boron amide alkane reducing agent is more expensive, the 2-3 that average unit cost is chemical nickel phosphorus plating times, and also technique is notMature and stable, so not yet heavy industrialization application at present.
By comprehensive comparison, chemical plating Nickel Phosphorus Alloy With High Phosphorus Content and carry out 400 DEG C/1h heat treatment be obtain high rigidity,The ideal technology of high abrasion aluminium alloy spare and accessory parts. If but part carries out 400 DEG C/1h heat treatment under antivacuum,Can coating make surface oxidation variable color (experimental data surface temperature exceedes 305 DEG C, coating will variable color), this is rightUnallowed in a lot of environments for use, if heat-treated under vacuum environment, so due to Vacuum HeatProcess expensive, the little space of stove and greatly limited again using and developing of this technique. Therefore, how existIn non-vacuum environment heat treatment, ensure that coating variable color does not occur and is oxidized and makes coating hardness to bring up to Hv >=850 to have veryLarge research space and Research Significance.
Summary of the invention
The object of this invention is to provide a kind of heat treatment method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer, non-trueUnder empty heat treated condition, improve hardness and the wearability of aluminum alloy surface chemical Ni-P layer.
A heat treatment method after Electroless Nickel Plating of Aluminum Alloy phosphorus alloy, its step is as follows:
1) aluminum alloy surface is carried out chemical plating nickel-phosphorus alloy.
2) aluminum alloy part that is coated with 10-14wt% nickel-phosphorus alloy coating is placed in to thermostatic drying chamber, is heated to200 DEG C, constant temperature 30min, then takes out, and air is cooling.
3) in boric acid spirit solution, add Sodium perfluorooctanoate as activating agent, after stirring, form heat treatment protectionAgent, puts into protective agent by the aluminum alloy part after drying, and soaks 5-10min, and soaking temperature is 20 DEG C-40 DEG C;
4) by soaking aluminum alloy part after heat treatment protective agent, to put into temperature be the Muffle furnace of 380 DEG C-450 DEG C,Constant temperature 40-60min heat treatment, then takes out, and air is cooling.
According to the present invention, described boric acid spirit solution, boric acid content is 4wt%.
According to the present invention, the Sodium perfluorooctanoate adding in described boric acid spirit solution is 1-5g/L.
Heat treatment method of the present invention, can ensure chemical nickel phosphorus plating (phosphorous 10-14% mass percent)Non-crystalline coating is after antivacuum heat treatment, and Hv >=850, and ensure that coating color does not change, with vacuumHeat treatment phase ratio, can be cost-saving, and break through the less limitation in vacuum drying oven space, expanded high phosphorus chemistryPlating nickel-phosphorus alloy, in the application on aluminum alloy part surface, has also expanded aluminium alloy at high performance requirements industrial circleApplication.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, but non-limitation of the present invention.
Embodiment 1:
The automobile valve core that 180 6061 rodss and bars of aluminium alloy are processed into carries out acidic chemical nickel phosphor plating and covers, chemistryNickel plating phosphorus plating technic parameter is pH value 4.5, nickel ion content 5.6g/L, 90 DEG C of temperature, time 100min.
Aluminum alloy part after 60 platings is placed in to thermostatic drying chamber, is heated to 200 DEG C, constant temperature 30min,Then take out, air is cooling; In the alcohol that is dissolved with 4wt% boric acid, add the Sodium perfluorooctanoate conduct of 1g/LActivating agent, forms heat treatment protective agent after stirring, and the aluminum alloy part after drying is put into protective agent, soaks5min, soaking temperature is 20 DEG C, it is 380 that the aluminum alloy part after immersion heat treatment protective agent is put into temperatureDEG C Muffle furnace, constant temperature 40min heat treatment, then take out, air is cooling.
As a comparison, the aluminum alloy part after 60 platings is directly put into R03 vacuum drying oven (vacuum10-2Pa) 380 DEG C of constant temperature 40min heat treatment, cooling with stove.
As a comparison, it is the Muffle furnace of 380 DEG C that the aluminum alloy part after 60 platings is directly put into temperature,Constant temperature 40min heat treatment, then takes out, and air is cooling.
Adopt XRF2000X ray layer thickness meter to measure thickness of coating, adopt HV1000 microhardness testersMeasurement coating hardness (test condition is: 50g, 15s, measures 3 some positions and averages), adopt InspectThe EDS energy spectrum analysis coating phosphorus content that F50 field emission scanning electron microscope is equipped with.
Test result is as shown in table 1:
Embodiment 2:
The automobile valve core that 180 6061 rodss and bars of aluminium alloy are processed into carries out acidic chemical nickel phosphor plating and covers, chemistryNickel plating phosphorus plating technic parameter is pH value 4.8, nickel ion content 5.8g/L, 90 DEG C of temperature, time 100min.
Aluminum alloy part after 60 platings is placed in to thermostatic drying chamber, is heated to 200 DEG C, constant temperature 30min,Then take out, air is cooling; In the alcohol that is dissolved with 4wt% boric acid, add the Sodium perfluorooctanoate conduct of 3g/LActivating agent, forms heat treatment protective agent after stirring, and the aluminum alloy part after drying is put into protective agent, soaks10min, soaking temperature is 40 DEG C, it is 450 that the aluminum alloy part after immersion heat treatment protective agent is put into temperatureDEG C Muffle furnace, constant temperature 50min heat treatment, then take out, air is cooling.
As a comparison, the aluminum alloy part after 60 platings is directly put into R03 vacuum drying oven (vacuum10-2Pa) 450 DEG C of constant temperature 50min heat treatment, cooling with stove.
As a comparison, it is the Muffle furnace of 450 DEG C that the aluminum alloy part after 60 platings is directly put into temperature,Constant temperature 50min heat treatment, then takes out, and air is cooling.
Adopt XRF2000X ray layer thickness meter to measure thickness of coating, adopt HV1000 microhardness testersMeasurement coating hardness (test condition is: 50g, 15s, measures 3 some positions and averages), adopt InspectThe EDS energy spectrum analysis coating phosphorus content that F50 field emission scanning electron microscope is equipped with.
Test result is as shown in table 2:
Embodiment 3:
The automobile valve core that 180 6061 rodss and bars of aluminium alloy are processed into carries out acidic chemical nickel phosphor plating and covers, chemistryNickel plating phosphorus plating technic parameter is pH value 4.7, nickel ion content 5.8g/L, 90 DEG C of temperature, time 100min.
Aluminum alloy part after 60 platings is placed in to thermostatic drying chamber, is heated to 200 DEG C, constant temperature 30min,Then take out, air is cooling; In the alcohol that is dissolved with 4wt% boric acid, add the Sodium perfluorooctanoate conduct of 5g/LActivating agent, forms heat treatment protective agent after stirring, and the aluminum alloy part after drying is put into protective agent, soaks8min, soaking temperature is 30 DEG C, it is 400 that the aluminum alloy part after immersion heat treatment protective agent is put into temperatureDEG C Muffle furnace, constant temperature 60min heat treatment, then take out, air is cooling.
As a comparison, the aluminum alloy part after 60 platings is directly put into R03 vacuum drying oven (vacuum10-2Pa) 400 DEG C of constant temperature 60min heat treatment, cooling with stove.
As a comparison, it is the Muffle furnace of 400 DEG C that the aluminum alloy part after 60 platings is directly put into temperature,Constant temperature 60min heat treatment, then takes out, and air is cooling.
Adopt XRF2000X ray layer thickness meter to measure thickness of coating, adopt HV1000 microhardness testersMeasurement coating hardness (test condition is: 50g, 15s, measures 3 some positions and averages), adopt InspectThe EDS energy spectrum analysis coating phosphorus content that F50 field emission scanning electron microscope is equipped with.
Test result is as shown in table 3:
Claims (3)
1. a heat treatment method for Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer, is characterized in that comprising the steps:
1) aluminum alloy part that is coated with nickel-phosphorus alloy coating is placed in to thermostatic drying chamber, is heated to 200 DEG C, constant temperature 30min, thenTake out, air is cooling, and wherein in nickel-phosphorus alloy coating, the content of phosphorus is 10-14wt%;
2) in boric acid spirit solution, add Sodium perfluorooctanoate as activating agent, after stirring, form heat treatment protective agent, will dryRear aluminum alloy part immerses protective agent, soaks 5-10min, and soaking temperature is 20 DEG C-40 DEG C;
3) by soaking aluminum alloy part after heat treatment protective agent, to put into temperature be the Muffle furnace of 380 DEG C-450 DEG C, constant temperature 40-60min heat treatment, then takes out, and air is cooling.
2. the heat treatment method after a kind of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy according to claim 1, is characterized in that: instituteState boric acid spirit solution, boric acid content is 4wt%.
3. the heat treatment method after a kind of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy according to claim 1, is characterized in that: instituteStating the Sodium perfluorooctanoate adding in boric acid spirit solution is 1-5g/L.
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| CN105132660A (en) * | 2015-09-25 | 2015-12-09 | 尚成荣 | Heat processing method of foot-operated type sawing machine fixture |
| CN105087883A (en) * | 2015-09-25 | 2015-11-25 | 尚成荣 | Protective agent applicable to heat treatment for checking tool used for pedal type sawing machine |
| CN105238914A (en) * | 2015-09-25 | 2016-01-13 | 尚成荣 | Method for preparing thermal treatment protective agent for detecting tool for detection of foot-pedal sawing machine |
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| CN100392151C (en) * | 2003-05-09 | 2008-06-04 | 昭和电工株式会社 | Corrosion resistant material, and its production method |
| CN1603465A (en) * | 2004-08-31 | 2005-04-06 | 中国兵器工业第五九研究所 | Treatment process for synergistic fluoropolymer coating on magnesium and its alloy |
| CN101705480B (en) * | 2009-11-03 | 2012-05-23 | 燕山大学 | Chemical modification technology of chemical nickel phosphorus plating alloy coating |
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