CN105200470B - A kind of Cu Sn PTFE TiO2Composite bed and its plating forming method - Google Patents
A kind of Cu Sn PTFE TiO2Composite bed and its plating forming method Download PDFInfo
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- CN105200470B CN105200470B CN201510677025.XA CN201510677025A CN105200470B CN 105200470 B CN105200470 B CN 105200470B CN 201510677025 A CN201510677025 A CN 201510677025A CN 105200470 B CN105200470 B CN 105200470B
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Abstract
The present invention is to provide a kind of Cu Sn PTFE TiO2Composite bed and its plating forming method.Nanometer polytetrafluoroethylcomposite obtains polytetrafluoroethyldispersion dispersion, nano-TiO in being distributed to nonionic surfactant2Colloidal dispersion obtains TiO to cationic surfactant2Colloidal dispersion agent, is heated to Cu Sn plating solutions 40~60 DEG C and keeps constant temperature to stir, and polytetrafluoroethyldispersion dispersion is slowly added to thereto at the temperature of stabilization, is slow added into TiO2Colloidal dispersion agent, forms electroplate liquid, surface treated metal works is electroplated in the electroplate liquid and forms Cu Sn PTFE TiO2Composite bed.In the form of dispersion liquid be added in composite plating bath PTFE by the present invention, by TiO2During composite plating bath is added in the form of the colloidal sol.By TiO2Dispersion-strengthened action, prepare the Cu Sn PTFE TiO of excellent performance2Composite deposite.
Description
Technical field
The present invention relates to a kind of self-lubricating layer, specifically a kind of Cu-Sn-PTFE-TiO2Composite bed.The present invention
It is directed to a kind of Cu-Sn-PTFE-TiO2The electro-plating method of composite bed.
Background technology
Friction is inevitable phenomenon in plant equipment operating, and friction makes energy be dissipated in the form of heat, and this makes
Into the substantial amounts of energy and the wasting of resources.The harm of friction is not only waste of resource, and friction causes the material of contact surface to wear and tear, makes
Mechanical operating part gradually loses precision, stability and reliability, or even causes equipment failure.Therefore, reduce friction and mitigate
Abrasion is always the unremitting research of numerous scholars and the problem explored.
Signal bronze is conventional wear resistant friction reducing material, is had a wide range of applications in sliding bearing.But in vacuum, low
Under some extreme conditions such as temperature, high temperature, the good lubrication of equipment cannot be just realized using common grease lubrication, equipment component has
Dry condition may be for a long time in, the huge abrasion of equipment is not only caused, and influence being normally carried out for production.
PTFE (polytetrafluoroethylene (PTFE)) is the minimum material of coefficient of friction in known friction material, and it is in self-lubricating coating
Using greatly being paid attention to.PTFE is high-molecular organic material, with long-chain banded structure, and is crystalline lamella and non-knot
Brilliant part is alternately arranged, and non-crystallized part is easily slided, and makes it have extremely low coefficient of friction, while also there is lacking for easy abrasion
Fall into.
Be compounded with the Cu-Sn-PTFE composite deposites of PTFE particles, by material in itself or its transfer membrane low sheraing characteristic
And there is excellent wear-resistant and antifriction function, lubrication problem of the sliding bearing under DRY SLIDING is solved to a certain extent.
For example in aviation turbofan engine with supercharger, many structures need to use oscillating bearing to ensure its function of realizing needing.
But harsh environment requires that it must possess good self-lubricating property, by its coating surface Cu-Sn-PTFE Composite Coatings
Layer, solves self-lubricating this problem.But due to soft, the easy to wear characteristic of PTFE matter, cause Cu-Sn-PTFE Composite Coatings
The layer defect that hardness is low, anti-wear performance is poor.And because PTFE specific grain surfaces product and surface can be all larger, in the plating solution easily
Agglomerate is gathered into, uniformly and stably dispersion becomes extremely difficult in the plating solution to make it.PTFE makes it because of having many advantages, such as
As the irreplaceable anti-corrosion of other materials and friction material.But meanwhile, the defect and deficiency that PTFE is present also limit it
Extensive use.
Nano-TiO2It is one of most common nano material, because it has good chemical stability, dispersiveness, machinery
Reinforcing property, ultraviolet screener effect is strong, and receives much concern.Sol-gal process is that one kind prepares nano-TiO2Mode, by chemical combination
Thing mixes under liquid phase, is hydrolyzed, is condensed chemical reaction, is prepared into stable transparent colloidal dispersion, then forms gel, passes through
Nano-scale is prepared in sintering, drying.Sol-gal process prepares nanoparticle to be influenceed by many factors, temperature, pH value,
Each composition combined amount etc., all influences success or failure, colloidal stability, the formation gel time of reaction.
The content of the invention
It is an object of the invention to provide one kind with wear-resistant, coefficient of friction is small, microhardness is high, compactness good, comprehensive
Close the Cu-Sn-PTFE-TiO of function admirable2Composite bed.The present invention also aims to provide a kind of Cu-Sn-PTFE-TiO2It is multiple
Close the plating forming method of layer.
Cu-Sn-PTFE-TiO of the invention2Composite bed, is to contain copper, tin, polytetrafluoroethylene (PTFE) and TiO2Four kinds of materials are answered
Layer is closed, the mass percent in the composite bed shared by each element is respectively Cu 80%~92%, Sn 4%~11%, F 2%
~3%, Ti 0.5%~1%.
Cu-Sn-PTFE-TiO of the invention2The plating forming method of composite bed is：
Nanometer polytetrafluoroethylcomposite obtains polytetrafluoroethyldispersion dispersion, nano-TiO in being distributed to nonionic surfactant2It is molten
Glue is distributed to cationic surfactant and obtains TiO2Colloidal dispersion agent, is heated to Cu-Sn plating solutions 40~60 DEG C and keeps permanent
Temperature stirring, polytetrafluoroethyldispersion dispersion is slowly added at the temperature of stabilization thereto, is slow added into TiO2Colloidal dispersion agent,
Form electroplate liquid,
Surface treated metal works are electroplated in the electroplate liquid and forms Cu-Sn-PTFE-TiO2Composite bed,
The electroplating technique condition is：35~45 DEG C of temperature, mechanical agitation rotating speed is 100~200r/min, and pH value is 9~10, electricity
Manifold formula is pulse current, and current density is 1.5~3.5A/dm2, dutycycle is 35%~85%, and frequency is 50~5000Hz.
Cu-Sn-PTFE-TiO of the invention2The plating forming method of composite bed can also include：
1st, polytetrafluoroethylene (PTFE) addition is 1~40g/L.
2、TiO2Colloidal sol addition is 1~120ml/L.
3rd, the main component and content in the Cu-Sn plating solutions are potassium pyrophosphate (K4P2O7·3H2O) 250~270g/L,
Cupric pyrophosphate (Cu2P2O7) 20~25g/L, sodium potassium tartrate tetrahydrate (KNaC4H4O6·4H2O) 30~35g/L, sodium stannate (Na2SnO3·
3H2O) 40~50g/L, potassium nitrate (KNO3) (40~45) g/L, sodium citrate (Na3C6H5O7·2H2O) (20~25) g/L.
In the form of dispersion liquid be added in composite plating bath PTFE by the present invention, and its advantage is than finished product PTFE emulsion
More preferably, process is simple, coating evenly, are conducive to improving the combination property of coating to dispersion effect.By TiO2In the form of colloidal sol
It is added in composite plating bath, its advantage compares nano-TiO2The dispersion effect of powder more preferably, can obtain more uniform multiple
Close coating.By TiO2Dispersion-strengthened action, prepare the Cu-Sn-PTFE-TiO of excellent performance2Composite deposite, solves mesh
The defect that preceding Cu-Sn-PTFE composite deposites hardness is low, anti-wear performance is poor.
Galvanoplastic prepare Cu-Sn-PTFE-TiO2Composite deposite has two outstanding features：1. by preparing PTFE points
Dispersion liquid, colloidal sol TiO2Form, obtain favorable dispersibility, the uniform composite plating bath of composition.2. nano-TiO is passed through2Dispersion-strengtherning
Effect, obtains the Cu-Sn-PTFE-TiO that abrasion resistance properties are excellent, coefficient of friction is low, compactness good, corrosion resistance is good2Composite Coatings
Layer.Can solve under some special operation conditions, lubrication problem of the sliding bearing under DRY SLIDING, the research and application of this respect
There is not relevant report also.
The present invention have found a kind of novel electroplating method, by preparing PTFE (polytetrafluoroethylene (PTFE)) dispersion liquid, colloidal sol TiO2
Form, prepare with wear-resistant, coefficient of friction it is small, microhardness is high, compactness good, the Cu-Sn- of high comprehensive performance
PTFE-TiO2Composite deposite, solves at present in some extreme condition properties of journal bearing lubricated such as vacuum, low temperature, high temperature well
Self-lubricating problem, while also providing a kind of simple to operate, low cost, pollution-free, safe electro-plating method.
The present invention prepares Cu-Sn-PTFE-TiO by electro-plating method2Composite deposite.Coating is in metallic element table
One layer of face plating contains copper, tin, PTFE (polytetrafluoroethylene (PTFE)), TiO2Four kinds of composite deposites of material, its advantage is raising
The wear resistance of coating, microhardness, reduction coefficient of friction.
Cu-Sn-PTFE-TiO of the invention2Electro-plating method, includes substrate pretreatment, and the preparation of plating solution is tried after plating
The post processing of sample.Including be plated the polishing of matrix, ultrasonic washing, alkali cleaning oil removing, washing, quickly dry up, weigh, pickling, washing,
Maceration extract is electroplated during electroplate liquid is put into after soaking.Test specimen after plating take out after with deionized water rinsing, be placed in alcohol
Be cleaned by ultrasonic, repeat this step 3 all over, quickly dry up, weigh, place into alcohol be cleaned by ultrasonic, quickly dry up after immediately
It is put into drying box.Its advantage is respectively the adhesion between enhancing matrix and coating, coating is given full play to it
The residue of excellent properties and removal matrix surface plating solution, prevents other materials pollution coating surface in air, influences it to detect
Effect.
Main salt is mantoquita (cupric pyrophosphate) and pink salt (sodium stannate) in Cu-Sn plating solutions, and sodium potassium tartrate tetrahydrate serves as in the plating solution
The role of auxiliary complex-former, potassium nitrate is the depolarizing agent commonly used in electroplating, and can reduce the polarization of negative electrode, improves the electricity of negative electrode
The current density upper limit.
The PTFE dispersion liquids of preparation, are, by nanoscale PTFE powder, powder to be divided using nonionic surfactant
Dissipate and obtain., first be put into for Cu-Sn plating solutions 40~60 DEG C be heated in water-bath by the method for adding PTFE dispersion liquids, and taking-up is placed on
On magnetic stirring apparatus, constant temperature stirring is kept, rotating speed 300r/min is then slow thereto at the temperature of stabilization to add PTFE
Dispersion liquid, continues to stir 5~10min after PTFE dispersion liquids are added and finished, and it is fully dissolved.
Nano-TiO2Colloidal sol is obtained by sol-gel process, and colloidal sol is disperseed using cationic surfactant.Plus
Enter nano-TiO2, first be put into for Cu-Sn plating solutions 40~60 DEG C be heated in water-bath by method, and taking-up is placed on magnetic stirring apparatus,
Constant temperature stirring is kept, rotating speed 300r/min is then slow thereto at the temperature of stabilization to add nano-TiO2Colloidal dispersion
Liquid, treats TiO2Sol dispersion adds and continues to stir 5~10min after finishing, and it is fully dissolved.
The present invention is due to using pulse plating method, water-soluble Cu-Sn-PTFE-TiO2Plating solution, addition is easily prepared
The PTFE dispersion liquid good with dispersion effect and nano-TiO2Colloidal sol, finally obtains Cu-Sn-PTFE-TiO2Composite deposite, this method
Have the advantages that can complex-curved plating, plating bath pollution-free, be easy to large-scale production, this method obtain coating have it is wear-resisting
Damage excellent performance, coefficient of friction is low, corrosion resistance is good, compactness is good, thickness is uniform and easily controllable, pin-free bubble the advantages of.
Brief description of the drawings
Fig. 1 is Cu-Sn-PTFE-TiO2Picture of the composite deposite under surface sweeping Electronic Speculum.
Fig. 2 (a)-Fig. 2 (b) is Cu-Sn-PTFE-TiO2Composite deposite EDS energy spectrum diagrams and each element percentage composition.
Fig. 3 is Cu-Sn-PTFE-TiO2Composite deposite friction coefficient curve figure.
Specific embodiment
Illustrate below and the present invention is described in more detail.
Embodiment 1：The plating Cu-Sn-PTFE-TiO on carbon tool steel2The method of composite deposite, including plated matrix
Polishing, use CW series water-proof abrasive papers to polish test specimen in this experimental technique, the sand paper trade mark is by slightly to carefully successively
It is 320 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1200 mesh, when changing next trade mark, wallpaper blade is along last time polishing direction
It is rotated by 90 °, the polishing scratch for being polishing to a trade mark sand paper is completely covered, and the trade mark is increased successively.Ultrasound is carried out after the completion of polishing
Washing 5min, takes out matrix, puts it into oil removing in alkali wash water, and alkali wash water is put into 75 DEG C of constant temperature in water-bath, heating 25
~30min.Then by matrix deionized water rinsing, then quick drying, it is weighed, record numerical value and be put into matrix
To in pickle, the time is 30s, washing, finally puts it into maceration extract immersion 30s, and being put into after taking-up in electroplate liquid carries out electricity
Plating.Main component and content in electroplate liquid are potassium pyrophosphate (K4P2O7·3H2O) 266g/L, cupric pyrophosphate (Cu2P2O7)20g/
L, sodium potassium tartrate tetrahydrate (KNaC4H4O6·4H2O) 30g/L, sodium stannate (Na2SnO3·3H2O) 40g/L, potassium nitrate (KNO3) 40g/L,
Sodium citrate (Na3C6H5O7·2H2O) 20g/L, PTFE powder 15g/L, TiO2Colloidal sol 40ml/L.Setting technological parameter, plating temperature
It is 38 DEG C to spend, and mechanical agitation rotating speed is 100r/min, and pH value is 9.5, and current forms are pulse current, and current density is 2.5A/
dm2, dutycycle is 60%, and frequency is 2000Hz, and electroplating time is 60min.Take out and use deionized water immediately after test specimen after electroplating
Rinse, being then placed in alcohol carries out ultrasonic cleaning 3min, repeat this step 4 time, in quickly drying up, weigh, placing into alcohol
It is immediately placed in drying box after ultrasonic cleaning, quick drying.It is obtained with the Cu- that wear-resistant, coefficient of friction is low, corrosion resistance is good
Sn-PTFE-TiO2Composite deposite.
Then with ESEM to Cu-Sn-PTFE-TiO2Composite deposite carries out Analysis of Surface Topography, and we can from Fig. 1
To find out, coating surface is bright and clean smooth, and crystal grain is uniform, reunites without large area, the phenomenon such as pin-free steam bubble.Fig. 2 (a) is Composite Coatings
The EDS energy spectrum diagrams of layer, it can be seen that the Elemental redistribution in coating substantially.The quality percentage of each element in coating is understood by Fig. 2 (b)
Number is respectively copper 90.83%, tin 6.35%, F 2.09%, Ti 0.72%.Fig. 3 is that composite deposite contacts unlubricated friction in ball disc type point
The coefficient of friction variation diagram under testing is wiped, the material to grinding steel ball is 60Cr, objective table rotating speed is 200r/min, and imposed load is
100g, the testing time is 10 minutes.
Exemplary description is done to the present invention above, it should which explanation, embodiments of the present invention are not limited to
Described above, as long as around core content of the invention, some simple modifications are carried out on its basis or are replaced all should
It is considered as protection scope of the present invention.
Claims (2)
1. a kind of Cu-Sn-PTFE-TiO2The plating forming method of composite bed, it is characterized in that：
Nanometer polytetrafluoroethylcomposite obtains polytetrafluoroethyldispersion dispersion, nano-TiO in being distributed to nonionic surfactant2Colloidal sol point
It is scattered to cationic surfactant and obtains TiO2Colloidal dispersion agent, is heated to Cu-Sn plating solutions 40~60 DEG C and keeps constant temperature to stir
Mix, polytetrafluoroethyldispersion dispersion is slowly added to thereto at the temperature of stabilization, be slow added into TiO2Colloidal dispersion agent, forms
Electroplate liquid, polytetrafluoroethylene (PTFE) addition is 1~40g/L, TiO2Colloidal sol addition is 1~120ml/L,
Surface treated metal works are electroplated in the electroplate liquid and forms Cu-Sn-PTFE-TiO2Composite bed, the electricity
The process conditions of plating are：35~45 DEG C of temperature, mechanical agitation rotating speed is 100~200r/min, and pH value is 9~10, current forms
It is pulse current, current density is 1.5~3.5A/dm2, dutycycle is 35%~85%, and frequency is 50~5000Hz.
2. Cu-Sn-PTFE-TiO according to claim 12The plating forming method of composite bed, it is characterized in that：The Cu-
Main component and content in Sn plating solutions are 250~270g/L of potassium pyrophosphate, 20~25g/L of cupric pyrophosphate, sodium potassium tartrate tetrahydrate 30
~35g/L, 40~50g/L of sodium stannate, 40~45g/L of potassium nitrate, 20~25g/L of sodium citrate.
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|---|---|---|---|---|
| CN104694997A (en) * | 2015-03-13 | 2015-06-10 | 哈尔滨工程大学 | Method for obtaining nano Cu-Sn-graphite composite coating and Cu-Sn-graphite electroplating solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104694997A (en) * | 2015-03-13 | 2015-06-10 | 哈尔滨工程大学 | Method for obtaining nano Cu-Sn-graphite composite coating and Cu-Sn-graphite electroplating solution |
Non-Patent Citations (4)
| Title |
|---|
| Production of Cu–Sn–graphite–SiC composite coatings by electrodeposition;Majid Asnavandi et al.;《Surface & Coatings Technology》;20121128;第207-214页 * |
| TiO2纳米粒子对Ni - PTFE 镀层微观组织结构和性能的影响研究;应丽霞等;《功能材料》;20150630;第46卷(第6期);06031-06034页 * |
| 焦磷酸盐低锡青铜合金电镀工艺及辅助配位剂的功能;冯绍彬;《材料保护》;20110831;第44卷(第8期);第34-37页 * |
| 电沉积铜/锡基复合层的摩擦学性能;顾卡丽等;《材料保护》;19970430;第30卷(第4期);第27-28页 * |
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