CN106119814A - A kind of Electroless Plating Ni P, surface self-lubricating technology of Ni P PTFE composite coating on pyrite - Google Patents
A kind of Electroless Plating Ni P, surface self-lubricating technology of Ni P PTFE composite coating on pyrite Download PDFInfo
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- CN106119814A CN106119814A CN201610687360.2A CN201610687360A CN106119814A CN 106119814 A CN106119814 A CN 106119814A CN 201610687360 A CN201610687360 A CN 201610687360A CN 106119814 A CN106119814 A CN 106119814A
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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
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1637—Composition of the substrate metallic substrate
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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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1662—Use of incorporated material in the solution or dispersion, e.g. particles, whiskers, wires
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- Chemically Coating (AREA)
Abstract
A kind of Electroless Plating Ni P, surface self-lubricating technology of Ni P PTFE composite coating on pyrite, first by matrix surface polishing, after ultrasonic waves for cleaning, brass base is carried out the pre-treating technology of electrochemical deoiling, acid-wash activation, the concentration of PTFE in the sedimentation time of control Ni P layer and N P PTFE plating solution, the final N P PTFE coating that obtains is as self-lubricating layer, and the minimized friction coefficient of the composite coating obtained is up to 0.161.Owing in the sedimentation time of Ni P layer of appropriateness and N P PTFE plating solution, PTFE concentration can provide more preferable sedimentary condition for Ni P PTFE composite coating; the performance making Ni P PTFE composite coating optimizes further; simultaneously because the excellent corrosion resistance of Ni P PTFE composite coating; this coating can be as the protective coating of rub resistance abrasion workpiece, and the method technique of the present invention is simple, deposition velocity fast, low cost, bond strength are good.
Description
Technical field
The invention belongs to Material Field, relate to a kind of metal surface modification lubricant coating, a kind of at pyrite specifically
The method of upper plating Ni-P, Ni-P-PTFE composite coating.
Background technology
The friction and wear of material all occurs at material surface, and the frictional behaviour therefore improving component of machine surface is one
Plant cost-effective technological means.In recent decades, sufacing is as a kind of method improving material surface performance, by people
Growing interest.Studying from material surface, improving anti-wear performance has two kinds of approach: one is that research has good mechanical properties
Surface modifying material and process means；Two is the rubbing surface (such as graphite, molybdenum bisuphide etc.) that research has nonmetal character
Friction and wear behavior and methods for using them.In all multi objective of mechanical property, the performance ginseng the closest with fretting wear relation
Number is hardness, and in most of the cases wear rate all can reduce with the raising of hardness, at present for improving material surface hardness
Research have been achieved for a lot of achievement.But high rigidity is not to affect the single factor of wearability, and high rigidity often carries
Carry out high coefficient of friction.From the basic theories of tribology, the coefficient of friction of material to be reduced and wear rate, it is necessary for making material
The surface of material has high rigidity and low shear strength simultaneously.In fact being difficult to obtain the homogenous material of this performance, this can only lead to
Cross the thin film of one layer of low shear strength of preparation on the matrix of high rigidity to realize.This thin film material to be advantageously reduced
Coefficient of friction, but also must can stop directly contact of material surface micro-bulge and mating plate, increase loaded area, make
It is perpendicular to the orthogonal shearing stress at the compressive stress of line of travel and contact point all reduce, thus suppresses contact area crack initiation,
Reducing the wear rate of material, our this coating material is called antifriction material.
Antifriction material is the lubricant particles adding Dispersed precipitate in coating material, such as graphite, MoS2Deng, its purpose
Being to reduce sliding frictional wear by the coefficient of friction of reduction friction pair, this type coating the most also has good
Antifriction quality, is therefore also called self-lubricating composite coating.In terms of existing document, with Metal Substrate or ceramic base Integral self-lubricating material phase
Ratio, it is simple that coating material has preparation technology, low cost, it is adaptable to the advantages such as the workpiece of various sizes, thus grinding at material
Critical role is occupied in studying carefully and developing.Multilamellar multiple component structure and gradient-structure can preferably suppress the shortcoming of one pack system, logical
Cross the quality adding other phase to improve coating, optimize coating, it is thus achieved that more more preferable properties of solid self-lubricant coating than one pack system performance.Week
Quiet, Cao Xingjin et al. is by choosing the high-temperature nickel-base alloy with excellent high temperature performance and certain self-lubricating property as compound painting
Layer matrix material, uses plasma spraying technology to work out the high temperature lubricating coating with the splendid compatibility.Think that the compatibility is good
Reason be owing to the gradient-structure of coating is better than single layer structure, gradient-structure has relaxed the physical property difference of coat inside,
The hardness not only making coating obtains gentle transition, and makes the bond strength of coating be greatly improved.
At present, it is combined politef (PTFE) codeposition of WC particles to chemical Ni-P plating coating is formed Ni-P-PTFE
Coating is most widely used, and PTFE has good chemical stability, excellent non-stick and high and low temperature resistance, especially
It is friction factor (friction factor is about 0.05) that this material is minimum than having with other polymer phases and is paid attention to.Due to
Ni-P-PTFE solid lubricant film has self-lubricating and anti-attrition function, thus substantially increases service life and the complete machine of parts
Work efficiency, decrease maintenance trouble.Therefore, the Ni-P-PTFE composite coating utilizing chemically plating standby has widely should
Use market.In research field, the preparation technology of Ni-P-PTFE composite coating has done excessive quantifier elimination.Such as, Liu Xuezhong,
The superfine electroless plating technology of Lee prepares the nano amorphous coating of Ni-P and Ni-P-PTFE at steel surface.Zhang Qingle, pay to have passed etc. and grind
Study carefully in plating solution activating agent and PTFE content to PTFE content, the impact of coating scaling rate in composite deposite.Fu Chuanqi, Wang Di etc.
Research surfactant and nano PTFE are on Ni-P-PTFE coating mechanics and the impact of tribological property.But, to Ni-P-
PTFE composite coating be the PTFE granule how realized in its self-lubricating property and Ni-P-PTFE composite coating how be shadow
Ring Ni-P-PTFE composite coating self-lubricating property we and be unaware of.We only really understand Ni-P-PTFE all sidedly
The self lubrication mechanism of composite coating, preferably could damage performance applications to work by the low friction, wear resistant of Ni-P-PTFE composite coating
Industry produces and in life.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of chemical Ni-P plating, Ni-P-on pyrite
The surface self-lubricating technology of PTFE composite coating, the described this method plating Ni-P, Ni-P-PTFE on pyrite to solve existing
There is the technical problem that the wear resistance of Brass coating in technology is the best.
The invention provides a kind of method plating Ni-P, Ni-P-PTFE on pyrite, comprise the steps:
1) brass substrate is put in acetone, use ultrasonic waves for cleaning；
2) first using chemical method that matrix carries out oil removing, then recycling hydrochloric acid solution carries out acid-wash activation；Needed for electrochemical deoiling
Solution in containing NaOH, Na2CO3 、Na3PO4, in described solution, the concentration of NaOH is 60-80g/L, Na2CO3's
Concentration is 20-60g/L, Na3PO4Concentration be 15-30g/L, solution is heated to 70-80 DEG C, then matrix is joined oil removing
In solution, the oil removing time is 10-15min, so that the greasy dirt of matrix surface is divided；
3) on base material, layer of Ni-P is plated, as transition zone by chemical plating；The pH value of Ni-P plating solution is 4.8, Ni-P plating solution
Temperature is 90 DEG C, and sedimentation time is 15min；
4) on Ni-P layer, Ni-P-PTFE layer is plated, as self-lubricating layer by chemical plating；Chemical Ni-P plating-PTFE plating solution dense
Degree is 50ml/L, and pH value is 4.8；Ni-P-PTFE bath temperature is 80 DEG C.
Further, in step 1), at described employing acetone on matrix, brass base surface is carried out ultrasound wave clear
Wash；Will put in the container containing acetone soln by base material, submergence, then container is positioned in ultrasonic washing instrument, power sets
Being set to 90w, set of time is 30min, oil removing organic to base material, it is thus achieved that clean matrix surface.
Further, step 2) in, the volume fraction of hydrochloric acid solution is 40-60%, and the matrix through oil removing is soaked hydrochloric acid
Carrying out acid-wash activation in solution, solution temperature is room temperature, and soak time is 3-5min so that the oxide layer quilt on brass base surface
Remove, obtain the brass substrate being completely exposed, allow the surface activity of matrix be greatly enhanced, the deposition of the most following Ni-P layer.
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating on pyrite of the present invention, be
First plate Ni-P layer on brass substrate as transition zone, then on Ni-P layer, plate Ni-P-PTFE layer as self-lubricating layer.Described
Double coatings are prepared first by matrix surface polishing, after ultrasonic waves for cleaning, brass base is carried out suitable electrochemical deoiling,
The pre-treating technology of acid-wash activation, in the sedimentation time of control Ni-P layer and N-P-PTFE plating solution, the concentration of PTFE, finally obtains
N-P-PTFE coating is as self-lubricating layer, and its minimized friction coefficient of the Ni-P-PTFE composite coating obtained is up to 0.161.Special
It not when during the sedimentation time of transition zone Ni-P layer is 15min, Ni-P-PTFE plating solution, the concentration of PTFE obtains when being 50ml/L
Ni-P-PTFE self-lubricating coat in use, coating microstrueture is finer and close, uniform.
Owing to PTFE concentration in the sedimentation time of Ni-P layer of appropriateness and N-P-PTFE plating solution can be compound for Ni-P-PTFE
Coating provides more preferable sedimentary condition so that the performance of Ni-P-PTFE composite coating optimizes further, simultaneously because Ni-P-
The excellent corrosion resistance of PTFE composite coating, this coating can be as the protective coating of rub resistance abrasion workpiece, its preparation side
Method has the advantages such as technique is simple, deposition velocity fast, low cost, bond strength are good.
The present invention compares with prior art, and its technological progress is significant.The present invention uses chemically plating for Ni-P, Ni-
The substrate surface self-lubrication treatment technology of the double coating of P-PTFE, by optimizing preparation technology parameter, prepares and has excellent rubbing
Wipe polishing machine and surface uniform Ni-P-PTFE self-lubricating coat in use.Compared with traditional handicraft, decrease the complexity of technique,
Reducing production cost, the friction and wear behavior of coating is improved simultaneously.
Accompanying drawing explanation
Fig. 1 be embodiment 2-6 in plating process in Ni-P-PTFE plating solution the concentration of PTFE be 40ml/L, Ni-P layer
Sedimentation time be respectively gained Ni-P-PTFE composite coating under 5min, 10min, 15min, 20min and 25min XRD spectrum
Figure；
Fig. 2 a is that PTFE concentration is 40ml/L, the chemistry of gained with the sedimentation time of the Ni-P layer in plating process as 5min
The Ni-P-PTFE self-lubricating coat in use surface topography SEM figure of plating；
Fig. 2 b be with the sedimentation time of the Ni-P layer in plating process as 10min, PTFE concentration as 40ml/L, the chemistry of gained
The Ni-P-PTFE self-lubricating coat in use surface topography SEM figure of plating；
Fig. 2 c be with the sedimentation time of the Ni-P layer in plating process as 15min, PTFE concentration as 40ml/L, the chemistry of gained
The Ni-P-PTFE self-lubricating coat in use surface topography SEM figure of plating；
Fig. 2 d be with the sedimentation time of the Ni-P layer in plating process as 20min, PTFE concentration as 40ml/L, the chemistry of gained
The Ni-P-PTFE self-lubricating coat in use surface topography SEM figure of plating；
Fig. 2 e be with the sedimentation time of the Ni-P layer in plating process as 25min, PTFE concentration as 40ml/L, the chemistry of gained
The Ni-P-PTFE self-lubricating coat in use surface topography SEM figure of plating；
Fig. 3 be embodiment 2-6 in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the heavy of 40ml/L, Ni-P layer
The long-pending time is respectively hardness and the friction of gained Ni-P-PTFE composite coating under 5min, 10min, 15min, 20min and 25min
Charts for finned heat；
Fig. 4, the embodiment 7-10 sedimentation time of Ni-P layer in plating process is that the concentration of 15min, PTFE is respectively 10ml/
The XRD spectra of the Ni-P-PTFE self-lubricating coat in use of gained under L, 30ml/L, 50ml/L, 70ml/L；
Fig. 5 a is that in plating process, the sedimentation time of Ni-P layer is that the concentration of 15min, PTFE is respectively gained under 10ml/L
The surface topography SEM figure of Ni-P-PTFE self-lubricating coat in use；
Fig. 5 b is that in plating process, the sedimentation time of Ni-P layer is that the concentration of 15min, PTFE is respectively gained under 30ml/L
The surface topography SEM figure of Ni-P-PTFE self-lubricating coat in use；
Fig. 5 c is that in plating process, the sedimentation time of Ni-P layer is that the concentration of 15min, PTFE is respectively gained under 50ml/L
The surface topography SEM figure of Ni-P-PTFE self-lubricating coat in use；
Fig. 5 d is that in plating process, the sedimentation time of Ni-P layer is that the concentration of 15min, PTFE is respectively gained under 70ml/L
The surface topography SEM figure of Ni-P-PTFE self-lubricating coat in use；
Fig. 6 be the sedimentation time of the layer of Ni-P in plating process as 15min, the concentration of PTFE be respectively 10ml/L, 30ml/L,
The hardness of the Ni-P-PTFE self-lubricating coat in use of gained and friction coefficient curve figure under 50ml/L, 70ml/L.
Detailed description of the invention
Below by specific embodiments and the drawings, the present invention is described in further detail, but is not limiting as the present invention.
Preparation, sign and measuring instrument used by the present invention:
In various embodiments of the present invention, the pre-nickel plating of gained uses the D8 ADVANCE type X-ray diffraction of Bruker company
(XRD) crystal phase structure of instrument analysed film；
The microcosmic of pre-nickel plating is analyzed with QuantaFEG450 type Flied emission environmental scanning electron microscope (SEM) of FEI Co.
Pattern and thickness；
Use Agilent company of the U.S. to produce NANO Indenter G200 type nano-hardness tester and measure the hardness of composite coating；
The fretting wear system of composite coating is measured with the HSR-2M reciprocating friction friabilator of Lanzhou Zhong Ke Hua Kai Science and Technology Ltd.
Number；
Embodiment 1
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating on pyrite, its preparation process include as
Lower step:
(1), by matrix putting in the beaker turned equipped with 100mL acetone, use ultrasonic waves for cleaning 10min, power setting is 90W；
(2), then using chemical method that matrix carries out oil removing, oil removing temperature is 70-80 DEG C, and the time is 10-15min, recycling
The hydrochloric acid of volume fraction 40-60% carries out acid-wash activation 3-5min to base material；
(3), utilizing chemical plating to plate Ni-P layer on brass base, as transition zone, bath temperature is 90 DEG C, plating process
The pH value of middle plating solution controls 4.8；Then plating Ni-P-PTFE layer on Ni-P layer, bath temperature is 80 DEG C, in plating process
The pH value of plating solution controls 4.8.
Using base material is H68 pyrite sample, and a length of 30mm, a width of 25mm, thickness is 0.3mm.
In above-mentioned plating process, controlling Ni-P bath temperature is 90 DEG C, and pH value is 4.8, and plating 15min obtains Ni-P
Layer；Controlling Ni-P-PTFE bath temperature is 80 DEG C, and pH value is 4.8, continues plating 30min and obtain Ni-P-PTFE on Ni-P layer
Layer, obtains Ni-P-PTFE self-lubricating coat in use after completing, including matrix, Ni-P layer and Ni-P-PTFE composite coating, it is from lower
On be followed successively by matrix Ni-P layer and Ni-P-PTFE composite coating.
Embodiment 2
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 50ml/L, Ni-P layer be 5min,
Using base material is H90 pyrite.
The other the same as in Example 1.
Embodiment 3
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 50ml/L, Ni-P layer be 10min,
Using base material is H70 pyrite.
The other the same as in Example 1.
Embodiment 4
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 50ml/L, Ni-P layer be 15min,
Using base material is H80 pyrite.
The other the same as in Example 1.
Embodiment 5
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 50ml/L, Ni-P layer be 20min,
Using base material is H68 pyrite.
The other the same as in Example 1.
Embodiment 6
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 50ml/L, Ni-P layer be 25min,
Using base material is H59 pyrite.
The other the same as in Example 1.
Embodiment 7
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 10ml/L, Ni-P layer be 15min,
Using base material is H68 pyrite.
The other the same as in Example 1.
Embodiment 8
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 30ml/L, Ni-P layer be 15min,
Using base material is H70 pyrite.
The other the same as in Example 1.
Embodiment 9
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 50ml/L, Ni-P layer be 15min,
Using base material is H59 pyrite.
The other the same as in Example 1.
Embodiment 10
A kind of surface self-lubricating technology of chemical Ni-P plating, Ni-P-PTFE composite coating, simply step of preparation process on pyrite
Suddenly in (3) in plating process in Ni-P-PTFE plating solution the concentration of PTFE be the sedimentation time of 70ml/L, Ni-P layer be 15min,
Using base material is H80 pyrite.
The other the same as in Example 1
In sum, the present invention obtains Ni-P-PTFE self-lubricating coat in use by electroless plating technology, and by controlling suitableization
Learn the concentration of PTFE in the Ni-P sedimentation time during plating and plating solution, final prepare a kind of obtained by electroless plating technology
Ni-P-PTFE self-lubricating coat in use, coating structure is fine and close, size uniform, and self-lubricating property is excellent.
Further, a kind of surface self-lubricating skill of chemical Ni-P plating, Ni-P-PTFE composite coating on pyrite of the present invention
Art, it is easy to industrialized production, production cost reduces.
Respectively in embodiment 2-6 i.e. plating process, in Ni-P-PTFE plating solution, PTFE concentration is 50ml/L, Ni-P layer
Sedimentation time respectively 5min, 10min, 15min, 20min and 25min under the Ni-P-PTFE composite coating of gained carry out XRD
Spectrogram measures, and result is as it is shown in figure 1, from figure 1 it appears that from Fig. 3 it is observed that different Ni-P layer sedimentation time
In XRD figure spectrum, occur that the position of 16 ° Ni occur in the diffraction maximum of PTFE, the position of 45 °3The diffraction maximum of P, the position of 72 ° occurs
Ni3S2Diffraction maximum.Increase (5min-15min) along with Ni-P layer sedimentation time, it is simply that the thickness of Ni-P layer increases, PTFE shape
The crystal diffraction peak become gradually is strengthening, Ni3The diffraction maximum of P is also gradually strengthening, but amplification is inconspicuous, Ni3" the steamed bread that P presents
Bag " diffraction maximum is the non crystalline structure of typical Ni-P alloy coat, enhances the hardness of coating.When the thickness of Ni-P layer is further
Increasing (15min-25min), the crystal diffraction peak that PTFE is formed gradually is weakening, Ni3The diffraction maximum of P is also weakening,
Ni3S2The intensity of diffraction maximum do not change significantly.
It is 50ml/L to the concentration of PTFE in embodiment 2-6 i.e. chemical Ni-P plating-PTFE plating solution respectively, chemical Ni-P plating
During the sedimentation time of Ni-P layer be respectively under 15min, 10min, 15min, 20min, 25min the Ni-P-PTFE of gained from
Lubricant coating, the surface topography SEM figure of gained is respectively as shown in Fig. 2 a, Fig. 2 b, Fig. 2 c, Fig. 2 d and Fig. 2 e, by Fig. 2 a, figure
2b, Fig. 2 c, Fig. 2 d and Fig. 2 e contrasts, and the sedimentation time of Ni-P-PTFE is controlled at 30min, along with Ni-P layer by experiment
The increase of sedimentation time, increases to the thickness of 25min, Ni-P layer from 5min and is constantly becoming big, and the thickness of Ni-P-PTFE layer in
The trend of existing first increases and then decreases.When the thickness of Ni-P layer increases to 1.597 m from 0.619 m, the thickness of Ni-P-PTFE layer
Degree also increases to 3.974 m from 1.100 m；When the thickness of Ni-P layer continues to thicken, when 1.597 m increase to 3.310 m,
The thickness of Ni-P-PTFE layer there will be thinning trend on the contrary, drops sharply to 0.6995 m from 3.974 m.Ni-P-PTFE layer
Deposit thickness occur that the reason of so change is: as Ni-P layer sedimentation time too short (5min), it is thus achieved that Ni-P layer ratio relatively thin
And uneven so that form the crystal grain arrangement defective tightness of Ni-P layer, but along with the prolongation (10-15min) of sedimentation time, Ni-P
Layer will more have an opportunity to reach state in uniform thickness, be 15min at sedimentation time, i.e. when Ni-P thickness is 1.597 m, and Ni-P layer
Thickness reach optimum state, tissue grainiess is compacted fine and closely woven further, creates for the chemical Ni-P plating-PTFE after Ni-P layer
Strong sedimentary condition so that composite coating is preferably deposited on Ni-P layer, PTFE is evengranular is distributed in Ni-P-PTFE
In composite coating, the interpretation of result with the XRD diffraction pattern of Fig. 1 Ni-P-PTFE composite coating is consistent.If but deposition
Overlong time (20-25min), the quality of plating solution itself declines due to consumption, causes portion of tissue particle coarsening, Ni-P layer table
The energy value everywhere in face is inconsistent, causes the sedimentary condition of chemical Ni-P plating-PTFE to be deteriorated, and Ni-P-PTFE layer is hardly formed,
So that the thickness of Ni-P-PTFE composite coating starts drastically to decline, the microcosmic that simultaneously can cause Ni-P-PTFE composite coating is brilliant
Grain cause not of uniform size, structure is sparse, and the gap between crystal grain becomes big so that Ni-P-PTFE composite coating and the combination of Ni-P layer
Intensity reduces, and the hardness of Ni-P-PTFE composite coating also decreases, and the roughness of coating surface also increases, and coefficient of friction increases
Greatly, self-lubricating property declines.
From the variation tendency of the SEM figure of Fig. 2 a, Fig. 2 b, Fig. 2 c, Fig. 2 d and Fig. 2 e it can be seen that its with Fig. 1 Electroless Plating Ni-
In P-PTFE plating solution, the concentration of PTFE is 50ml/L, during chemical Ni-P plating the sedimentation time of Ni-P layer be respectively 15min,
The XRD spectra of the Ni-P-PTFE composite coating that 10min, 15min, 20min, 25min obtain is consistent.
It is 50ml/L to the concentration of PTFE in embodiment 2-6 i.e. chemical Ni-P plating-PTFE plating solution respectively, chemical Ni-P plating mistake
The Ni-P-PTFE that in journey, the sedimentation time of Ni-P layer respectively 15min, 10min, 15min, 20min, 25min obtain is compound to be coated with
Coefficient of friction and the hardness of layer carry out test and are measured, and fit to hardness and friction coefficient curve as it is shown on figure 3, from Fig. 3
Curve in can be seen that understand, when deposited between during 5min increases to 25min, Ni-P-PTFE composite coating
The trend that coefficient of friction quickly increases after occurring first being gradually reduced, hardness occurs first strengthening the trend drastically reduced afterwards.In deposition
When time is 15min, it is 0.161 that the coefficient of friction of Ni-P-PTFE composite coating minimizes value；Hardness reaches maximum
4.548GPa.
We combine Fig. 1 and Fig. 2 and comprehensively analyze the self lubrication mechanism of Ni-P-PTFE composite coating and changed by Ni-P thickness and affected
Trend.First, when Ni-P layer thickness increases to 1.597 m from 0.619 m, as shown in Fig. 2 (a) and (b), (c), Ni-P layer
Thickness progressivelyes reach the state of an even compact, is especially advantageous for the deposition of Ni-P-PTFE layer, significantly more efficient formation Ni-P-
PTFE composite coating, makes the networked pore structures the most more even compact of Ni-P-PTFE composite coating, and PTFE granule is wrapped equably
It is rolled in networked pore structures.Meanwhile, as shown in the XRD diffracting spectrum of Fig. 3 Ni-P-PTFE composite coating, PTFE granule is in deposition
Time is 15min, i.e. thickness when being 1.597 m, and the crystalline state of its crystal grain is best, and PTFE granule is distributed more in composite coating
Uniformly, grain shape is more tiny, and the densification that is evenly distributed of the reticulated cell on Ni-P-PTFE composite coating surface, so working as Ni-P
When the sedimentation time of layer is 15min, composite coating obtains hardness and reaches to be to the maximum 4.548GPa, coefficient of friction minimum 0.161,
The self-lubricating property of Ni-P-PTFE composite coating is best.When the thickness of Ni-P layer continues to thicken, increase to 3.310 from 1.597 m
During m, as shown in Fig. 2 (d), (e), along with Ni-P layer sedimentation time increases (20-25min) further, the quality of plating solution itself by
Declining in consumption, cause portion of tissue particle coarsening, the energy value everywhere on Ni-P layer surface is inconsistent so that chemical plating
The sedimentary condition of Ni-P-PTFE is deteriorated, and is unfavorable for the formation of Ni-P-PTFE composite coating.Simultaneously multiple according to Fig. 3 Ni-P-PTFE
Closing shown in the XRD diffracting spectrum of coating, in composite coating, the degree of crystallinity of PTFE granule is deteriorated, and the cause not of uniform size of crystal grain causes
The empty structure size of the reticulated cell of Ni-P-PTFE composite coating is inconsistent, and structure is sparse so that Ni-P-PTFE composite coating
Hardness decrease, when coating surface contacts with object plane, owing to hardness is low, surface is easily worn, and according to from
Lubricant coating mechanism, the PTFE lubricated granules being extruded out is due to cause not of uniform size, it is impossible to is evenly distributed in contact surface, leads
The wearability causing coating is deteriorated, so that the self-lubricating property of Ni-P-PTFE composite coating is greatly reduced.
It is that 15min, PTFE concentration is divided respectively to the sedimentation time of Ni-P layer during embodiment 7-10 i.e. chemical Ni-P plating
Wei not carry out X-ray diffraction spectrum survey by the Ni-P-PTFE self-lubricating coat in use of gained under 10ml/L, 30ml/L, 50ml/L and 70ml/L
Fixed, result such as result as shown in Figure 4, figure 4, it is seen that the XRD of the Ni-P-PTFE composite coating under difference PTFE concentration
In diffracting spectrum, occur that the position of 16 ° Ni occur in the diffraction maximum of PTFE, the position of 45 °3The diffraction maximum of P, the position of 72 ° goes out
Existing Ni3S2Diffraction maximum.Along with the increase (10-50ml/L) of PTFE concentration, the crystal diffraction peak that PTFE is formed gradually is strengthening,
Ni3The diffraction maximum of P is also gradually strengthening, but amplification is inconspicuous." steamed bread bag " diffraction maximum that Ni3P presents is that typical Ni-P closes
The diffraction maximum of the non crystalline structure of gold plating, enhances the hardness of coating.When PTFE concentration increases (50-70ml/L) further,
The crystal diffraction peak that PTFE is formed is weakening, Ni3The diffraction maximum of P has weakened, Ni3S2The intensity of diffraction maximum the brightest
Aobvious change.
It is that 15min, PTFE concentration is divided respectively to the sedimentation time of Ni-P layer during embodiment 7-10 i.e. chemical Ni-P plating
Wei not sweep by the surface topography of the Ni-P-PTFE self-lubricating coat in use of gained under 10ml/L, 30ml/L, 50ml/L and 70ml/L
Retouching, the surface topography SEM figure of gained, as shown in Fig. 5 a, Fig. 5 b, Fig. 5 c and Fig. 5 d, is carried out by Fig. 5 a, Fig. 5 b, Fig. 5 c, Fig. 5 d
Contrast, along with PTFE concentration increases, black splotch gradually increases, and is that 50ml/L makes black splotch most in PTFE concentration, from
When 50ml/L increases to 70ml/L, black splotch gradually decreases again.It is understood that Ni-P-PTFE composite coating is a kind of reticulated cell
Structure, Ni-P alloy coat forms a kind of reticulated cell, and PTFE granule is wrapped in Ni-P alloy coat reticulated cell, so we
The black splotch observed is exactly the PTFE granule wrapped up of composite coating networked pore structures.Thus we can obtain, with
PTFE concentration to increase, PTFE granule is more evenly distributed in composite coating, and grain shape is more tiny, composite coating surface
The densification that is evenly distributed of reticulated cell, when PTFE concentration is 50ml/L, the microstructure of composite coating reaches optimal.When PTFE is dense
When degree increases further, the PTFE distribution of particles that composite coating networked pore structures is wrapped up just becomes uneven, and shape size is poor
Different bigger, a certain amount of ground caking phenomenon occurs, the reticulated cell of formation is also distributed sparse.
Respectively to embodiment 7-10 the most respectively to the sedimentation time of Ni-P layer during embodiment 7-10 i.e. chemical Ni-P plating
The Ni-P-PTFE self-lubricating coat in use of gained under 10ml/L, 30ml/L, 50ml/L and 70ml/L it is respectively for 15min, PTFE concentration
Case hardness and coefficient of friction be measured, and fit to curve as shown in Figure 6, as can be drawn from Figure 6, along with PTFE is dense
The increase of degree, the hardness of composite coating presents first to reduce to be increased afterwards, then the trend reduced, and when PTFE concentration is 10ml/L, reaches
To maximum 4.908GPa.The coefficient of friction of composite coating then presents and first reduces the trend increased afterwards, is 50ml/ in PTFE concentration
During L, it is 0.16 that coefficient of friction minimizes.We combine Fig. 4 and Fig. 5 and analyze, although there is Ni at 45 °3P diffraction maximum strong
Spend the change with PTFE concentration little, but the hardness of composite coating is affected the most clearly.This be primarily due to along with
The increase of PTFE concentration, causes the plot ratio of PTFE granule in Ni-P-PTFE composite coating to increase, and PTFE granule is a kind of
Soft phase particle, when composite coating surface imposed load, surface is susceptible to plastic deformation.When composite coating is along with PTFE concentration
Increase, hardness is reducing, this is because PTFE granule disperses wider in composite coating, plot ratio increases so that compound be coated with
The effective area of layer surface Ni-P alloy reduces, and causes coating hardness to decline.When PTFE concentration increases to 50ml/L from 30ml/L,
Hardness has risen and has been because when PTFE concentration is 50ml/L, the more tiny cause of networked pore structures that composite coating is formed
Close, PTFE distribution of particles obtains evenly because PTFE granule is wrapped around in reticulated cell, so with apply power physical contact surface
Long-pending less, bear the main still Ni-P alloy coat surface of load, so hardness has raised.When PTFE concentration increases from 50ml/L
When being added to 70ml/L, the PTFE distribution of particles that composite coating networked pore structures is wrapped up just becomes uneven, shape size difference
Bigger, a certain amount of ground caking phenomenon occurs, the reticulated cell of formation is also distributed sparse so that the ratio that the hardness of composite coating reduces
More apparent.
Comprehensively analyze also according to Fig. 4 and Fig. 5 (a) and (b), (c), (d), along with the increase of PTFE concentration, composite coating
In XRD figure spectrum, PTFE forms the trend weakened after diffraction peak intensity presents enhancing, shows in composite coating, when PTFE concentration is
During 50ml/L, the crystal structure of formation is best.Self lubrication mechanism according to self-lubricating coat in use can be learnt, when composite coating surface with
During body surface generation phase mutual friction, friction process can produce amount of heat, here it is frictional heat, it and compressive stress one act as
With, the kollag being in self-lubricating layer top layer can be made to squeeze out top layer, under frictionization dynamic action, PTFE granule quilt
Pullling, form stable chemical bond, along with the carrying out of friction, a large amount of PTFE granules are extruded out, are slowly smoothed covering and exist
Tie layer surface, form PTFE lubricating film.PTFE lubricating film prevents the effective contact between friction pair effectively, no matter rubs
It is to form complete lubricating film between wiping face, or forming part lubricating film all can play the effect of antifriction.So, when PTFE concentration
When 10ml/L increases to 50ml/L, in composite coating, PTFE granule is more evenly distributed in the networked pore structures of composite coating
In, the reticulated cell more fine uniform that composite coating surface is formed, when there is friction with body surface in composite coating, PTFE
Grain is more prone to be extruded top layer, forms uniform lubricating film, thus is substantially reduced the friction and wear behavior of composite coating, with
Time, this networked pore structures makes Ni-P-PTFE composite coating can preferably be engaged with Ni-P layer, greatly increase coating it
Between bond strength.So, the self lubricity of Ni-P-PTFE composite coating reaches optimal when PTFE concentration is 50ml/L.When
When PTFE concentration increases further, due to PTFE concentration in Ni-P-PTFE plating solution excessive time, can cause PTFE granule plating
Disperseing the most uneven in liquid, cause the PTFE granule dispersion wrapped up in composite coating network structure uneven, shape size is poor
Different relatively big, the reticulated cell of formation is the most sparse, cause not of uniform size, so when friction, the PTFE granule being " squeezed. " out
Not being easily formed uniform lubricating film, the self-lubricating property eventually causing composite coating surface reduces, and friction and wear behavior is weak.
By above example, it is achieved that by changing sedimentation time and the PTFE concentration of the Ni-P layer in plating process, enter
The one-step optimization technique preparing Ni-P-PTFE composite coating: the sedimentation time of the Ni-P layer in plating process is 15min；
PTFE concentration is 50ml/L.Under this technique, the Ni-P-PTFE composite coating structure of preparation is fine and close, even grain size, coating
And it is tightly combined between matrix, surface self-lubricating best performance.
Above said content is only the basic explanation under present inventive concept, and according to appointing that technical scheme is made
What equivalent transformation, all should belong to protection scope of the present invention.
Claims (3)
1. a chemical Ni-P plating on pyrite, the surface self-lubricating technology of Ni-P-PTFE composite coating, it is characterised in that include
Following steps:
1) brass substrate is put in acetone, use ultrasonic waves for cleaning；
2) first using chemical method that matrix carries out oil removing, then recycling hydrochloric acid solution carries out acid-wash activation；Needed for electrochemical deoiling
Solution in containing NaOH, Na2CO3 、Na3PO4, in described solution, the concentration of NaOH is 60-80g/L, Na2CO3's
Concentration is 20-60g/L, Na3PO4Concentration be 15-30g/L, solution is heated to 70-80 DEG C, then matrix is joined oil removing
In solution, the oil removing time is 10-15min, so that the greasy dirt of matrix surface is divided；
3) on base material, layer of Ni-P is plated, as transition zone by chemical plating；The pH value of Ni-P plating solution is 4.8, Ni-P plating solution
Temperature is 90 DEG C, and sedimentation time is 15min；
4) on Ni-P layer, Ni-P-PTFE layer is plated, as self-lubricating layer by chemical plating；Chemical Ni-P plating-PTFE plating solution dense
Degree is 50ml/L, and pH value is 4.8；Ni-P-PTFE bath temperature is 80 DEG C.
A kind of surface self-lubricating skill of chemical Ni-P plating, Ni-P-PTFE composite coating on pyrite
Art, it is characterised in that:
In step 1), at the described acetone that uses on matrix, brass base surface is carried out ultrasonic waves for cleaning；Will put by base material
Enter in the container containing acetone soln, submergence, then container is positioned in ultrasonic washing instrument, power setting is 90w, and the time sets
It is set to 30min, oil removing organic to base material, it is thus achieved that clean matrix surface.
A kind of surface self-lubricating skill of chemical Ni-P plating, Ni-P-PTFE composite coating on pyrite
Art, it is characterised in that:
Step 2) in, the volume fraction of hydrochloric acid solution is 40-60%, is soaked in hydrochloric acid solution by the matrix through oil removing and carries out acid
Washing activation, solution temperature is room temperature, and soak time is 3-5min so that the oxide layer on brass base surface is removed, and has obtained
The full brass substrate exposed, allows the surface activity of matrix be greatly enhanced, the deposition of the most following Ni-P layer.
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| CN110656325A (en) * | 2019-08-27 | 2020-01-07 | 江苏大学 | Ni-P-nano TiO on copper alloy surface2Composite plating solution preparation and plating process |
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| CN113981424A (en) * | 2021-09-24 | 2022-01-28 | 宁波博威合金材料股份有限公司 | Chemical plating Ni-P-graphene composite coating and preparation method thereof |
| CN113981424B (en) * | 2021-09-24 | 2023-09-12 | 宁波博威合金材料股份有限公司 | Chemical plating Ni-P-graphene composite coating and preparation method thereof |
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