CN105780081B - Prepare the electrolyte of arc differential oxide ceramic composite coating - Google Patents

Prepare the electrolyte of arc differential oxide ceramic composite coating Download PDF

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CN105780081B
CN105780081B CN201610259080.1A CN201610259080A CN105780081B CN 105780081 B CN105780081 B CN 105780081B CN 201610259080 A CN201610259080 A CN 201610259080A CN 105780081 B CN105780081 B CN 105780081B
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electrolyte
arc oxidation
composite coating
coating
sodium
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CN105780081A (en
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阎峰云
马颖
王晟
孙文峰
陈体军
繆欢
刘洪军
曹驰
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Lanzhou University of Technology
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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
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/024—Anodisation under pulsed or modulated current or potential
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/26—Anodisation of refractory metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The invention discloses under three kinds of different systems, MoS is contained by differential arc oxidation preparation2The electrolyte prescription of composite coating, electrolyte are characterized under basic electrolyte system, and the sodium molybdate of 5 ~ 7g/L and the vulcanized sodium of 25 ~ 35g/L is added, passes through differential arc oxidation one-step synthesis MoS containing amorphous state2Ceramic composite coating, which makes the MoS in coating using 250 ~ 500 DEG C, the vacuum heat treatment of 1 ~ 4h of soaking time2Crystallization.The advantages of its method, is not only to maintain the high intensity and high rigidity of common micro-arc oxidation ceramic layer, but also increases the MoS organically combined with ceramic phase2Self-lubricating phase, hence it is evident that improve the wearability of coating；This method belongs to direct combination technology, and operating procedure is simple.

Description

Prepare the electrolyte of arc differential oxide ceramic composite coating
Technical field
The invention belongs to light metal surface process fields, are specially adapted to the differential of the arc oxygen of aluminium alloy, magnesium alloy, titanium alloy Change the preparation method and electrolyte prescription of Friction-Reducing Coating.
Background technique
Differential arc oxidization technique, also known as micro-plasma oxidation, anodic spark deposition or spark discharge anodic oxidation, this method are The non-ferrous metals such as Al, Mg, Ti or its alloy material are placed in special electrolyte solution, by of electrolyte and electrical parameter With adjusting, under the TRANSIENT HIGH TEMPERATURE high pressure effect that arc discharge generates, it is major-minor for growing in alloy surface with base oxide With the ceramic coating of electrolyte component.It can be according to different needs, the control size of output current density, electrolyte solution Component and concentration and oxidization time etc. obtain the ceramic coating formed by micro-arc oxidation of different performance, with meet the metals such as Al, Mg, Ti and The surface property requirement of alloy.So differential arc oxidization technique is a kind of rising process for treating surface.
Single differential arc oxidation method can make alloy surface form bond strength height, hard ceramic layer with high hardness, improve The surface hardness of alloy and the performances such as wear-resisting, anti-corrosion.In terms of the structure of differential arc oxidation coating, the microcosmic composition of coating is by porous Gap and hard a variety of ceramic phase compositions.Under the conditions of oil lubrication, micropore can have good antifriction to make with lubricant storage With.But under dry friction conditions, due to the effect of shaggy ceramic hard phase, not only without friction reducing effect, and easily The damage to membrane material is caused, although can improve frictional property by the method for polishing ceramic surface, this coating is without certainly Lubricant effect.With the raising of sliding workpiece requirement under large contacting stress environment, coefficient of friction to alloy surface and Wear-resisting property has harsher requirement, and simple differential arc oxidization technique is no longer satisfied requirement, needs to develop differential arc oxidation Composite coating technology, or the ceramic coating obtained to differential arc oxidation are for further processing, and to reduce its skin-friction coefficient, mention High-wearing feature.Mainly there are two aspects for research to differential arc oxidation composite coating technology at present and application, first is that in differential arc oxidation Self-lubricating solid particle (such as MoS is added in electrolyte2, the powder such as C, PTFE), capture this during micro-arc discharge sintering A little particles form composite layer；Second is that obtaining anti-attrition to surface second processing using techniques such as spraying, electrophoresis after differential arc oxidation Coating.In these above-mentioned methods, either particle is inlayed or surface coating, the combination of these self-lubricating materials and ceramic phase are equal For mechanical bond, it is be easy to cause particle and coating shedding, polishing machine deteriorates in the later period.
CN200810063913.2 discloses a kind of preparation side of aluminum alloy surface high abrasion anti-attrition self-lubricating composite coating Aluminium alloy after differential arc oxidation is placed in tetrafluoroethene lotion by method, is carried out in the environment of vacuum degree is 0.03~0.1MPa It is sucked by vacuum 10~60min, makes polytetrafluoroethylene (PTFE) micro-nano impregnation into micropore, to obtain a kind of composite coating.
CN201510519048.8 has handled pure magnesium sheet material by the addition graphene in basic electrolyte (silicic acid system), The thickness and consistency of coating are improved, occurs SiC phase in coating, coating hardness and frictional behaviour are improved.
Yan comes into et al. (a kind of structure of low-friction coefficient the compound lubricating film and performance study " aeronautical material journal " 2011,31 (5): 58-61) using differential arc oxidation and spraying molybdenum disulfide base lubricating material and in 150~200 DEG C of solidification 2h or so Technique, be prepared for the compound lubricating film of low-friction coefficient in aluminum alloy surface.Coating by differential arc oxidation obtain with γ- 50 μm of dense sclerosis layer based on Al2O3 and surface spray MoS210~15 μm of layer, shows the hardness and curing of ceramic layer The self-lubricating feature of molybdenum.Grey sky of Lee et al. (anti-attrition film layer " Chinese Foundry equipment of the aluminum alloy differential arc oxidation preparation containing molybdenum disulfide With technology ", 2015 (5): 54-57) by adding solid lubricant molybdenum disulfide particles in micro-arc oxidation electrolyte, in aluminium Alloy surface is directly prepared for the differential arc oxidation compound film layer containing molybdenum disulfide.The table of the layer of differential arc oxidation compound film containing molybdenum disulfide Face is more smooth compared with the common film surface of differential arc oxidation without molybdenum disulfide, and aperture is more tiny, and molybdenum disulfide is in film layer It is evenly distributed, coefficient of friction is small.
Summary of the invention
The purpose of the present invention is improving the excessively high problem of single differential arc oxidation coating coefficient of friction, one kind is researched and developed in differential of the arc oxygen While change forms ceramic phase, using metallurgy sintered and chemical reaction, while MoS containing self-lubricating phase is obtained2Method, formed MoS2The composite coating that self-lubricating phase and ceramic phase mix.
The electrolyte of arc differential oxide ceramic composite coating is prepared in the present invention, it is characterised in that: in the water-soluble of differential arc oxidation Property electrolyte in be added synthesis of carbon/molybdenum disulfide needed for Na2S and Na2MoO4, sulphion and molybdenum acid ion after hydrolysis are yin Ion can be adsorbed by anode under electrophoretic effect effect, and when micro-arc discharge occurs metallurgy sintered and chemical reaction, one-step synthesis and contains Self-lubricating phase MoS2Anti-attrition composite coating.
The invention discloses the electrolyte prescriptions of three kinds of different systems, which is characterized in that
(1) when prepared electrolyte is silicate, formula are as follows: 10~16g/L of sodium metasilicate, 1~4g/L of potassium fluoride, boron Acid 1~4g/L, 5~7g/L of sodium molybdate, 25~35g/L of vulcanized sodium, 5~7ml/L of glycerine；
(2) when prepared electrolyte is phosphate-based, formula are as follows: 8~14g/L of calgon, 3~7g/ of potassium fluoride L, 5~7g/L of sodium molybdate, 25~35g/L of vulcanized sodium；
(3) when prepared electrolyte is aluminate-series, formula are as follows: 10~16g/L of sodium aluminate, 2~6g/L of sodium hydroxide, 5~7g/L of sodium molybdate, 25~35g/L of vulcanized sodium.
The invention also discloses a kind of preparation methods of arc differential oxide ceramic composite coating, and its step are as follows:
(1) it is polished workpiece surface, oil removing and cleaning treatment；
(2) micro-arc oxidation electrolyte is configured, is put into electrolytic cell after mixing evenly；
(3) workpiece handled well is put into the electrolyte of preparation and carries out micro-arc oxidation treatment: workpiece connects anode, electrolyte Cathode is connect, is powered and carries out differential arc oxidation, 300~500V of final voltage, duty ratio 10%~40%, pulse frequency 200~ 1000Hz handles 20~100min of time；During entire micro-arc oxidation treatment, electrolyte temperature is controlled at 20~40 DEG C.
(4) workpiece after differential arc oxidation is taken out, rinses 5~10min with tap water flowing water, washes away remaining electrolyte, It is put into the drying box that temperature is 80~100 DEG C later, dries 1h；
(5) dried workpiece is placed in vacuum heat treatment furnace and is heat-treated, final workpiece surface is obtained containing pottery Porcelain phase and MoS2The composite coating that crystal is mutually mixed, coating layer thickness can achieve 10~60 μm.
The MoS in film layer after differential arc oxidation2For amorphous state, to strengthen MoS2Effect will be obtained in step (5) The workpiece of differential arc oxidation coating, which is placed in vacuum heat treatment furnace, carries out crystallization and thermal treatment, and temperature controls the heat preservation at 250~500 DEG C 1~4h of time.
Composite coating is prepared using electrolyte of the invention, compared to existing technology, its advantage is:
(1) it joined generation lubrication phase MoS in the electrolytic solution2Presoma, using it is metallurgy sintered and chemical reaction simultaneously Obtain MoS containing self-lubricating phase2Composite coating, coefficient of friction substantially reduces, and wearability improves；
(2) MoS of self-lubricating2It is mutually formed and is organically combined with ceramic phase, coating dense uniform is good with substrate combinating strength；Film Thick controllable, thickness is at 10~60 μm；One step of composite coating is formed, and preparation process is simple, easily operated；
(3) preparation method strong applicability of the invention, under silicate, phosphate and the various electrolyte systems of aluminate It can get the lower anti-attrition composite coating of coefficient of friction.
Specific embodiment
Example is enumerated below to illustrate the present invention.
Differential arc oxidation method: it is polished workpiece surface, the pretreatment such as oil removing and cleaning；Configure differential arc oxidation electrolysis Workpiece connect with power anode and is placed in electrolyte by liquid；Voltage is controlled in 300~500V, duty ratio 10%~40%, pulse 200~1000Hz of frequency handles 20~100min of time；It is crossed in engineering in entire micro-arc oxidation treatment, controls electrolyte temperature At 20~40 DEG C；Processed workpiece is taken out, is placed in drying box with tap water flushing dry；Workpiece is placed in Vacuum Heat It is heat-treated in treatment furnace, final workpiece surface is obtained containing ceramic phase and MoS2The composite coating that crystal is mutually mixed.
Embodiment 1:2219 aluminium alloy differential arc oxidation under silicate systems
Electrolyte prescription are as follows: sodium metasilicate 14g/L, potassium fluoride 3g/L, boric acid 4g/L, sodium molybdate 7g/L, vulcanized sodium 35g/L, Glycerol 5ml/L；The selection of electrical parameter: final voltage 450V, duty ratio 30%, frequency 600Hz handle time 45min；Heat treatment Temperature is 400 DEG C, keeps the temperature 3h.
The composite coating main component that the above method obtains is aluminum oxide, the curing of silica and 2H crystal form There is lubricating action the coefficient of friction of coating greatly reduces for molybdenum, molybdenum disulfide, and coating layer thickness is compared with common differential arc oxidation There is significant raising, coating layer thickness can achieve 35~40 μm.
Embodiment 2:2219 aluminium alloy differential arc oxidation under phosphate system
Electrolyte prescription are as follows: calgon 14g/L, potassium fluoride 6g/L, sodium molybdate 7g/L, vulcanized sodium 30g/L；Electrical parameter Selection: final voltage 450V, duty ratio 40%, frequency 500Hz, handle time 50min；Heat treatment temperature is 450 DEG C, heat preservation 2h。
The coating main component of acquisition is ceramic phase γ-Al2O3、α-Al2O3With the molybdenum disulfide of 2H crystal form, coating surface Dense uniform, roughness Ra=2.1 μm, coating layer thickness are 30~35 μm, and the molybdenum disulfide of 2H crystal form is uniformly distributed in the coating, So that coefficient of friction significantly reduces compared with matrix, stablize coefficient of friction between 0.3~0.4.
Embodiment 3:AZ91D magnesium alloy differential arc oxidation under phosphate system
Electrolyte prescription are as follows: calgon 12g/L, potassium fluoride 4g/L, sodium molybdate 6g/L, vulcanized sodium 30g/L；Electrical parameter Selection: final voltage 400V, duty ratio 25%, frequency 700Hz, handle time 40min；350 DEG C of heat treatment temperature, heat preservation 2h。
The main component for the composite coating that the above method obtains is MgO and MgAl2O4The molybdenum disulfide of spinelle, generation exists It is evenly distributed in coating；Coating layer thickness can achieve 30~35 μm.Coating surface is more smooth compared with common differential arc oxidation, hole Diameter is more tiny, has smaller coefficient of friction under dry friction conditions, stable coefficient of friction is between 0.2~0.3.
Embodiment 4:AZ91D magnesium alloy differential arc oxidation under silicate systems
Electrolyte prescription are as follows: sodium metasilicate 12g/L, potassium fluoride 2g/L, boric acid 2g/L, sodium molybdate 5g/L, vulcanized sodium 25g/L； The selection of glycerine 7ml/L electrical parameter: final voltage 400V, duty ratio 20%, frequency 600Hz handle time 35min；At heat 450 DEG C of temperature of reason keeps the temperature 3h.
The coating that above-mentioned formula obtains mainly contains the Mg of MgO, forsterite structure2SiO4、SiO2And the two of 2H crystal form Molybdenum sulfide, stable friction factor is 0.3~0.4.
Embodiment 5:Ti6Al4V titanium alloy differential arc oxidation under aluminates system
Electrolyte prescription are as follows: sodium aluminate 16g/L, sodium hydroxide 3g/L, sodium molybdate 6g/L, vulcanized sodium 30g/L；Electrical parameter Selection: final voltage 380V, duty ratio 15%, frequency 800Hz handle time 35min；350 DEG C of heat treatment temperature, keep the temperature 2h.
The composite coating main component that the above method obtains is rutile TiO2、Al2TiO5, 2H crystal form molybdenum disulfide and A small amount of γ-Al2O3, coating layer thickness can achieve 20~25 μm.Anti-attrition lubrication is played in the presence of molybdenum disulfide reduces coefficient of friction Effect, TiO2、Al2TiO5With γ-Al2O3The hardness and wearability of coating can be improved in the presence of equal hard phases, so that coating Friction and wear behavior significantly improve, abrasion loss be matrix 1/3.
Embodiment 6:Ti6Al4V titanium alloy differential arc oxidation under phosphate system
Electrolyte prescription are as follows: calgon 10g/L, potassium fluoride 3g/L, sodium molybdate 5g/L, vulcanized sodium 30g/L；Electrical parameter Selection: final voltage 400V, duty ratio 20%, frequency 800Hz, handle time 40min；400 DEG C of heat treatment temperature, heat preservation 2h。
Contain ceramic phase rutile TiO in the coating that above-mentioned formula obtains2With the molybdenum disulfide of lubrication phase 2H crystal form, surface Smooth, film thickness can achieve 25 μm；The molybdenum disulfide of 2H crystal form in coating is evenly distributed, and coefficient of friction significantly reduces, and stablizes Coefficient of friction is between 0.2~0.3.

Claims (5)

1. preparing the electrolyte of arc differential oxide ceramic composite coating, which is characterized in that
When prepared electrolyte is silicate, proportion and step are as follows: in distilled water, sequentially add 10~16g/ of sodium metasilicate L, 1~4g/L of potassium fluoride, 1~4g/L of boric acid, 5~7g/L of sodium molybdate, 25~35g/L of vulcanized sodium, 5~7ml/L of glycerine, to preceding A kind of reagent adds latter reagent after being completely dissolved, and dissolution is sufficiently stirred and stands 30 minutes；
Prepared electrolyte be it is phosphate-based when, proportion and step are as follows: in distilled water, sequentially add calgon 8~ 14g/L, 3~7g/L of potassium fluoride, 5~7g/L of sodium molybdate, 25~35g/L of vulcanized sodium add again after former reagent is completely dissolved Enter latter reagent, dissolution is sufficiently stirred and stands 30 minutes；
When prepared electrolyte is aluminate-series, proportion and step are as follows: in distilled water, sequentially add 10~16g/ of sodium aluminate L, 2~6g/L of sodium hydroxide, 5~7g/L of sodium molybdate, 25~35g/L of vulcanized sodium are added after former reagent is completely dissolved Latter reagent is sufficiently stirred dissolution and stands 30 minutes.
2. preparing the electrolyte of arc differential oxide ceramic composite coating as described in claim 1, characterized in that using institute respectively When stating phosphate system electrolyte, the phosphate-based electrolyte and the aluminate-series electrolyte, comprising the following steps:
(1) mechanical grinding, oil removing and cleaning is carried out to workpiece surface to pre-process；
(2) micro-arc oxidation electrolyte is poured into electrolytic cell；
(3) micro-arc oxidation treatment: the workpiece pre-processed is immersed in electrolyte, and workpiece jointed anode, electrolyte connects cathode, is led to Electricity carries out micro-arc oxidation treatment, handles 20~100min of time, and the thicknesses of layers of acquisition is 10~60 μm；
(4) workpiece after micro-arc oxidation treatment is taken out, rinses 5~10min with tap water flowing water, washes away remaining electrolyte, It is put into the drying box that temperature is 80~100 DEG C later, dries 1h；
(5) dried sample is placed in vacuum heat treatment furnace and is heat-treated, final workpiece surface is obtained containing ceramic phase And MoS2The composite coating that crystal is mutually mixed.
3. preparing the electrolyte of arc differential oxide ceramic composite coating as claimed in claim 2, characterized in that the step (1) material of the workpiece in is aluminium alloy, titanium alloy and magnesium alloy.
4. preparing the electrolyte of arc differential oxide ceramic composite coating as claimed in claim 2, characterized in that the step (5) in, heat treatment temperature controls 1~4h of soaking time between 250~500 DEG C.
5. preparing the electrolyte of arc differential oxide ceramic composite coating as claimed in claim 2, characterized in that the step (3) in, differential arc oxidation electrical parameter are as follows: 300~500V of final voltage, duty ratio 10%~40%, 200~1000Hz of pulse frequency, During entire micro-arc oxidation treatment, electrolyte temperature is controlled at 20~40 DEG C.
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CN106884192B (en) * 2017-03-07 2018-12-04 大连海事大学 A kind of preparation process of self-lubrication ceramic based composites
CN108468075A (en) * 2018-03-27 2018-08-31 杭州电子科技大学 A kind of electrolyte and its application process of differential arc oxidation self-lubricating composite ceramic coating
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