CN105200470A - Cu-Sn-PTFE (polytetrafluoroethylene)-TiO2 composite layer and electroplating forming method thereof - Google Patents

Cu-Sn-PTFE (polytetrafluoroethylene)-TiO2 composite layer and electroplating forming method thereof Download PDF

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CN105200470A
CN105200470A CN201510677025.XA CN201510677025A CN105200470A CN 105200470 A CN105200470 A CN 105200470A CN 201510677025 A CN201510677025 A CN 201510677025A CN 105200470 A CN105200470 A CN 105200470A
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ptfe
tio
composite bed
plating
dispersion
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CN105200470B (en
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应丽霞
吴珂
吕秀鹏
石洪瑞
朱腾飞
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Harbin Engineering University
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Harbin Engineering University
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Abstract

The invention provides a Cu-Sn-PTFE (polytetrafluoroethylene)-TiO2 composite layer and an electroplating forming method thereof. Nano PTFE is dispersed in a nonionic surfactant, and a PTFE dispersion solution is obtained; nano-TiO2 sol is dispersed in a cationic surfactant, and a TiO2 sol dispersion agent is obtained, a Cu-Sn plating solution is heated to 40-60 DEG C and stirred at the temperature, the PTFE dispersion solution is slowly added to the mixture at the stable temperature, the TiO2 sol dispersion agent is slowly added, an electroplating solution is formed, a metal workpiece subjected to surface processing is electroplated in the electroplating solution, and a Cu-Sn-PTFE-TiO2 composite layer is formed. The PTFE dispersion solution is added to the composite plating solution, TiO2 sol is added to the composite plating solution, and the Cu-Sn-PTFE-TiO2 composite layer with excellent performance is prepared through the dispersion strengthening function of TiO2.

Description

A kind of Cu-Sn-PTFE-TiO 2composite bed and plating formation method thereof
Technical field
What the present invention relates to is a kind of self-lubricating layer, specifically a kind of Cu-Sn-PTFE-TiO 2composite bed.The present invention also relates to a kind of Cu-Sn-PTFE-TiO 2the electro-plating method of composite bed.
Background technology
Friction is inevitable phenomenon in mechanical means running, and friction makes energy dissipate with the form of heat, and this causes a large amount of energy and the wasting of resources.Waste resource is not only in the harm of friction, and friction causes the fret wear of surface in contact, makes mechanical operating part lose precision, stability and reliability gradually, even causes equipment failure.Therefore, reduce friction and alleviate the problem that wearing and tearing are the unremitting research of numerous scholars and exploration always.
Gunmetal is conventional wear resistant friction reducing material, has a wide range of applications in sliding surface bearing.But under some extreme conditions such as vacuum, low temperature, high temperature, adopt common grease lubrication just cannot realize the good lubrication of equipment, equipment component is likely in dry condition for a long time, not only causes the huge wearing and tearing of equipment, and affects normally carrying out of production.
PTFE (tetrafluoroethylene) is the material that in known friction materials, frictional coefficient is minimum, and its application in self-lubricating coating is subject to great attention.PTFE is organic polymer material, has long-chain zonal structure, and is that crystalline lamella and non-crystallized part are alternately arranged, and non-crystallized part easily slides, and makes it have extremely low frictional coefficient, also has the defect of easily wearing and tearing simultaneously.
Be compounded with the Cu-Sn-PTFE composite deposite of PTFE particle, rely on the low sheraing characteristic of material itself or its transfer film and there is excellent wear-resistant and antifriction function, solving the lubrication problem of sliding surface bearing under DRY SLIDING to a certain extent.Such as in aviation turbofan engine with supercharger, many structures need to use oscillating bearing to ensure that it realizes the function of needs.But the environmental requirement of harshness its must possess good self-lubricating property, by its coating surface Cu-Sn-PTFE composite deposite, solve this difficult problem of self-lubricating.But because PTFE matter is soft, characteristic easy to wear, causes the defect that Cu-Sn-PTFE composite deposite hardness is low, wear resisting property is poor.And because PTFE specific grain surface sum surface energy is all comparatively large, be very easily gathered into agglomerate in the plating solution, make it disperse uniformly and stably in the plating solution to become very difficulty.PTFE becomes the irreplaceable anticorrosion and friction materials of other material because having plurality of advantages.But meanwhile, the defect that exists of PTFE and the not enough widespread use that also limit it.
Nano-TiO 2be one of modal nano material, because it has good chemical stability, dispersiveness, mechanical robustness, ultraviolet screener effect is strong, and receives much concern.Sol-gel method is that one prepares nano-TiO 2mode, compound is mixed under liquid phase, is hydrolyzed, condensation chemical reaction, be prepared into stable transparent colloidal dispersion, then form gel, prepare nano-scale by sintering, drying.Sol-gel method is prepared nanoparticle and is subject to many factors impact, and temperature, pH value, each composition combined amount etc., all affects the success or failure of reaction, colloidal stability, formation gel time.
Summary of the invention
The object of the present invention is to provide a kind of have wear-resistant, frictional coefficient is little, microhardness is high, compactness is good, the Cu-Sn-PTFE-TiO of high comprehensive performance 2composite bed.The present invention also aims to provide a kind of Cu-Sn-PTFE-TiO 2the plating formation method of composite bed.
Cu-Sn-PTFE-TiO of the present invention 2composite bed is containing copper, tin, tetrafluoroethylene and TiO 2the composite bed of four kinds of materials, the mass percent in described composite bed shared by each element is respectively Cu80% ~ 92%, Sn4% ~ 11%, F2% ~ 3%, Ti0.5% ~ 1%.
Cu-Sn-PTFE-TiO of the present invention 2the plating formation method of composite bed is:
Nanometer polytetrafluoroethylcomposite is distributed in nonionogenic tenside and obtains polytetrafluoroethyldispersion dispersion, nano-TiO 2colloidal dispersion obtains TiO to cats product 2colloidal dispersion agent, is heated to 40 ~ 60 DEG C by Cu-Sn plating solution and keeps constant temperature to stir, slowly adding polytetrafluoroethyldispersion dispersion wherein, more slowly add TiO at stable temperature 2colloidal dispersion agent, forms electroplate liquid,
Surface treated metal works is electroplated in described electroplate liquid and forms Cu-Sn-PTFE-TiO 2composite bed, described electroplating technique condition is: temperature 35 ~ 45 DEG C, and mechanical stirring rotating speed is 100 ~ 200r/min, and pH value is 9 ~ 10, and current forms is pulsed current, and current density is 1.5 ~ 3.5A/dm 2, dutycycle is 35% ~ 85%, and frequency is 50 ~ 5000Hz.
Cu-Sn-PTFE-TiO of the present invention 2the plating formation method of composite bed can also comprise:
1, tetrafluoroethylene addition is 1 ~ 40g/L.
2, TiO 2colloidal sol addition is 1 ~ 120ml/L.
3, the main component in described Cu-Sn plating solution and content are potassium pyrophosphate (K 4p 2o 73H 2o) 250 ~ 270g/L, cupric pyrophosphate (Cu 2p 2o 7) 20 ~ 25g/L, Seignette salt (KNaC 4h 4o 64H 2o) 30 ~ 35g/L, sodium stannate (Na 2snO 33H 2o) 40 ~ 50g/L, saltpetre (KNO 3) (40 ~ 45) g/L, Trisodium Citrate (Na 3c 6h 5o 72H 2o) (20 ~ 25) g/L.
PTFE joins in composite plating bath with the form of dispersion liquid by the present invention, and its beneficial effect is better than the dispersion effect of finished product PTFE emulsion, technique is simple, coating evenly, be conducive to the over-all properties improving coating.By TiO 2join in composite plating bath with the form of colloidal sol, its beneficial effect compares nano-TiO 2the dispersion effect of powder is better, can obtain more uniform composite deposite.Pass through TiO 2dispersion-strengthened action, prepare the Cu-Sn-PTFE-TiO of excellent performance 2composite deposite, solves the defect that current Cu-Sn-PTFE composite deposite hardness is low, wear resisting property is poor.
Electrochemical plating prepare Cu-Sn-PTFE-TiO 2composite deposite has two outstanding features: 1. by preparation PTFE dispersion liquid, colloidal sol TiO 2form, obtain favorable dispersity, the composite plating bath of uniform composition.2. nano-TiO is passed through 2dispersion-strengthened action, obtain abrasion resistance properties excellence, frictional coefficient be low, compactness good, Cu-Sn-PTFE-TiO that solidity to corrosion is good 2composite deposite.Under can solving some special operation conditions, the lubrication problem of sliding surface bearing under DRY SLIDING, the Study and appliance of this respect does not also have relevant report.
The present invention have found a kind of Novel electroplating method, by preparation PTFE (tetrafluoroethylene) dispersion liquid, and colloidal sol TiO 2form, prepare have wear-resistant, frictional coefficient is little, microhardness is high, compactness is good, the Cu-Sn-PTFE-TiO of high comprehensive performance 2composite deposite, well solves at present in the self-lubricating problem of some extreme condition properties of journal bearing lubricated such as vacuum, low temperature, high temperature, also provides a kind of simple to operate, electro-plating method that cost is low, pollution-free, safe simultaneously.
The present invention prepares Cu-Sn-PTFE-TiO by electro-plating method 2composite deposite.Coating is for contain copper, tin, PTFE (tetrafluoroethylene), TiO at metallic element coating surface one deck 2the composite deposite of four kinds of materials, its beneficial effect is the wearability, microhardness, the reduction frictional coefficient that improve coating.
Cu-Sn-PTFE-TiO of the present invention 2electro-plating method, includes substrate pretreatment, the preparation of plating solution, the aftertreatment of sample after plating.Comprise the polishing of plated matrix, ultrasonic washing, alkali cleaning oil removing, washing, dry up fast, weigh, pickling, washing, steeping fluid put into electroplate liquid and electroplate after soaking.Test specimen after plating takes out rear deionized water rinsing, be placed in alcohol carry out ultrasonic cleaning, repeat this step 3 time, dry up fast, weigh, put into alcohol ultrasonic cleaning again, dry up fast after put into loft drier immediately.Its beneficial effect is respectively the bonding force strengthened between matrix and coating, makes coating can give full play to its excellent properties and removes the residue of matrix surface plating solution, preventing other Substances Pollution coating surface in air, affect its Detection results.
In Cu-Sn plating solution, main salt is mantoquita (cupric pyrophosphate) and pink salt (sodium stannate), Seignette salt serves as the role of auxiliary complex-former in the plating solution, saltpetre is depolarizer conventional in plating, can reduce the polarization of negative electrode, improves the current density upper limit of negative electrode.
The PTFE dispersion liquid of preparation is by nano level PTFE powder, adopts nonionogenic tenside to carry out dispersion to powder and obtains.Add the method for PTFE dispersion liquid, first Cu-Sn plating solution is put into water-bath and be heated to 40 ~ 60 DEG C, taking-up is placed on magnetic stirring apparatus, constant temperature is kept to stir, rotating speed 300r/min, then at stable temperature, add PTFE dispersion liquid slowly wherein, treat that PTFE dispersion liquid continues stirring 5 ~ 10min after adding, make it fully dissolve.
Nano-TiO 2colloidal sol is obtained by sol-gel method, adopts cats product to disperse colloidal sol.Add nano-TiO 2method, first puts into water-bath by Cu-Sn plating solution and is heated to 40 ~ 60 DEG C, takes out and is placed on magnetic stirring apparatus, and keep constant temperature to stir, rotating speed 300r/min, then adds nano-TiO slowly wherein at stable temperature 2sol dispersion, treats TiO 2continue stirring 5 ~ 10min after sol dispersion adds, make it fully dissolve.
The present invention is owing to adopting pulse plating method, water-soluble Cu-Sn-PTFE-TiO 2plating solution, what add is be easy to prepare and the good PTFE dispersion liquid of dispersion effect and nano-TiO 2colloidal sol, finally obtains Cu-Sn-PTFE-TiO 2composite deposite, present method have can at complex-curved plating, plating bath pollution-free, be easy to the advantages such as scale operation, present method obtain coating has abrasion resistance properties excellence, frictional coefficient is low, solidity to corrosion good, compactness is good, thickness is even and be easy to the advantages such as control, free of pinholes bubble.
Accompanying drawing explanation
Fig. 1 is Cu-Sn-PTFE-TiO 2the picture of composite deposite under surface sweeping Electronic Speculum.
Fig. 2 (a)-Fig. 2 (b) is Cu-Sn-PTFE-TiO 2composite deposite EDS can spectrogram and each element percentage composition.
Fig. 3 is Cu-Sn-PTFE-TiO 2composite deposite friction coefficient curve figure.
Embodiment
Illustrate below and the present invention is described in more detail.
Embodiment 1: plating Cu-Sn-PTFE-TiO on carbon tool steel 2the method of composite deposite, comprise the polishing of plated matrix, CW series water-proof abrasive paper is used to polish to test specimen in this experimental technique, the sand paper trade mark is extremely carefully followed successively by 320 orders, 400 orders, 600 orders, 800 orders, 1000 orders, 1200 orders by thick, when changing next trade mark, wallpaper blade was polished along last time direction 90-degree rotation, and the polishing scratch of a supreme trade mark sand paper of polishing is completely covered, and increases the trade mark successively.Ultrasonic washing 5min to be carried out after having polished, take out matrix, put it into oil removing in alkaline wash, alkaline wash is put into constant temperature 75 DEG C in water-bath, heating 25 ~ 30min.Then by matrix deionized water rinsing, then dry up fast, weigh to it, matrix is also put in pickle solution by record numerical value, and the time is 30s, washing, finally puts it into steeping fluid and soaks 30s, put into electroplate liquid and electroplate after taking-up.Main component in electroplate liquid and content are potassium pyrophosphate (K 4p 2o 73H 2o) 266g/L, cupric pyrophosphate (Cu 2p 2o 7) 20g/L, Seignette salt (KNaC 4h 4o 64H 2o) 30g/L, sodium stannate (Na 2snO 33H 2o) 40g/L, saltpetre (KNO 3) 40g/L, Trisodium Citrate (Na 3c 6h 5o 72H 2o) 20g/L, PTFE powder 15g/L, TiO 2colloidal sol 40ml/L.Setting processing parameter, electroplating temperature is 38 DEG C, and mechanical stirring rotating speed is 100r/min, and pH value is 9.5, and current forms is pulsed current, and current density is 2.5A/dm 2, dutycycle is 60%, and frequency is 2000Hz, and electroplating time is 60min.Use deionized water rinsing immediately after test specimen after taking out plating, be then placed in alcohol and carry out ultrasonic cleaning 3min, repeat this step 4 time, dry up fast, weigh, put into alcohol ultrasonic cleaning again, dry up fast after put into loft drier immediately.Just can obtain wear-resistant, that frictional coefficient is low, solidity to corrosion is good Cu-Sn-PTFE-TiO 2composite deposite.
Then by scanning electron microscope to Cu-Sn-PTFE-TiO 2composite deposite carries out Analysis of Surface Topography, as can be seen from Fig. 1 we, coating surface is bright and clean smooth, uniform crystal particles, without big area reunite, the phenomenons such as free of pinholes steam bubble.The EDS energy spectrogram that Fig. 2 (a) is composite deposite, can find out Elemental redistribution roughly in coating.Copper 90.83% is respectively, tin 6.35%, F2.09%, Ti0.72% by the mass percent of each element in the known coating of Fig. 2 (b).Fig. 3 is the frictional coefficient variation diagram of composite deposite under ball disc type point cantact dry wear test, and be 60Cr to the material of mill steel ball, Stage microscope rotating speed is 200r/min, and applied load is 100g, and the test duration is 10 minutes.
Above to invention has been exemplary description; should be noted that; embodiments of the present invention are not limited to above-mentioned explanation, as long as around core content of the present invention, on its basis, carrying out some, simply amendment or replacement all should be considered as protection scope of the present invention.

Claims (6)

1. a Cu-Sn-PTFE-TiO 2composite bed, is characterized in that containing copper, tin, tetrafluoroethylene and TiO 2the composite bed of four kinds of materials, the mass percent in described composite bed shared by each element is respectively Cu80% ~ 92%, Sn4% ~ 11%, F2% ~ 3%, Ti0.5% ~ 1%.
2. a Cu-Sn-PTFE-TiO 2the plating formation method of composite bed, is characterized in that:
Nanometer polytetrafluoroethylcomposite is distributed in nonionogenic tenside and obtains polytetrafluoroethyldispersion dispersion, nano-TiO 2colloidal dispersion obtains TiO to cats product 2colloidal dispersion agent, is heated to 40 ~ 60 DEG C by Cu-Sn plating solution and keeps constant temperature to stir, slowly adding polytetrafluoroethyldispersion dispersion wherein, more slowly add TiO at stable temperature 2colloidal dispersion agent, forms electroplate liquid,
Surface treated metal works is electroplated in described electroplate liquid and forms Cu-Sn-PTFE-TiO 2composite bed, described electroplating technique condition is: temperature 35 ~ 45 DEG C, and mechanical stirring rotating speed is 100 ~ 200r/min, and pH value is 9 ~ 10, and current forms is pulsed current, and current density is 1.5 ~ 3.5A/dm 2, dutycycle is 35% ~ 85%, and frequency is 50 ~ 5000Hz.
3. Cu-Sn-PTFE-TiO according to claim 2 2the plating formation method of composite bed, is characterized in that: tetrafluoroethylene addition is 1 ~ 40g/L.
4. the Cu-Sn-PTFE-TiO according to Claims 2 or 3 2the plating formation method of composite bed, is characterized in that: TiO 2colloidal sol addition is 1 ~ 120ml/L.
5. the Cu-Sn-PTFE-TiO according to Claims 2 or 3 2the plating formation method of composite bed, is characterized in that: the main component in described Cu-Sn plating solution and content are potassium pyrophosphate (K 4p 2o 73H 2o) 250 ~ 270g/L, cupric pyrophosphate (Cu 2p 2o 7) 20 ~ 25g/L, Seignette salt (KNaC 4h 4o 64H 2o) 30 ~ 35g/L, sodium stannate (Na 2snO 33H 2o) 40 ~ 50g/L, saltpetre (KNO 3) (40 ~ 45) g/L, Trisodium Citrate (Na 3c 6h 5o 72H 2o) (20 ~ 25) g/L.
6. Cu-Sn-PTFE-TiO according to claim 4 2the plating formation method of composite bed, is characterized in that: the main component in described Cu-Sn plating solution and content are potassium pyrophosphate (K 4p 2o 73H 2o) 250 ~ 270g/L, cupric pyrophosphate (Cu 2p 2o 7) 20 ~ 25g/L, Seignette salt (KNaC 4h 4o 64H 2o) 30 ~ 35g/L, sodium stannate (Na 2snO 33H 2o) 40 ~ 50g/L, saltpetre (KNO 3) (40 ~ 45) g/L, Trisodium Citrate (Na 3c 6h 5o 72H 2o) (20 ~ 25) g/L.
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Publication number Priority date Publication date Assignee Title
CN108554371A (en) * 2018-05-16 2018-09-21 内江师范学院 A method of preparing silicon magnesium-base nano water treatment agent

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108554371A (en) * 2018-05-16 2018-09-21 内江师范学院 A method of preparing silicon magnesium-base nano water treatment agent
CN108554371B (en) * 2018-05-16 2020-11-17 内江师范学院 Method for preparing silicon-magnesium-based nano water treatment agent

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