CN106283162A - A kind of high temperature resistant composite deposite and preparation method thereof - Google Patents
A kind of high temperature resistant composite deposite and preparation method thereof Download PDFInfo
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- CN106283162A CN106283162A CN201610748875.9A CN201610748875A CN106283162A CN 106283162 A CN106283162 A CN 106283162A CN 201610748875 A CN201610748875 A CN 201610748875A CN 106283162 A CN106283162 A CN 106283162A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
The invention discloses the preparation method of a kind of refractory metal base composite cladding.Composite deposite is with cobalt as matrix metal, and the chromium carbide particles of nickel coated as dispersion phase, high-load and homodisperse chromium carbide particles, makes composite deposite all keep higher hardness under room temperature and high temperature.Composite plating bath is disperseed by the mode utilizing mechanical agitation and ultrasonic agitation, forms uniform and stable composite plating bath.The matrix of electro-deposition is metal material, first matrix surface is carried out pretreatment, by technological parameters such as the temperature of Comprehensive Control electro-deposition, electric current density, plating solution flow, anode and cathode relative moving speeds, makes metal Co and hard particles Cr3C2Codeposition, forms composite deposite.The present invention solves micron order hard particles during composite electrodeposition and is difficult to that high-load is compound, hard particles skewness and hard particles in coating are combined the problem of bad layer, prepared Co Cr with matrix metal Co3C2Composite deposite, has higher high temperature hardness and excellent wearability.
Description
Technical field
The present invention relates to composite electrodeposition technique field.
Background technology
Along with industrial expansion, material performance requirement is improved constantly, utilize surface coating technique that material surface is entered
The method of row strengthening and protection is the most industrially widely used, and electroplating technology is as a kind of surface coating technique, and it has
Have simple to operate, with low cost, pollute the little and molding advantage such as quickly, be widely used the most in the industrial production.
But traditional monometallic coating and alloy layer are difficult to meet the modern requirement to material surface high temperature protection, by matrix metal
Co-deposit, with insoluble hard particles, fiber etc., the composite deposite formed, because of it, there is the most excellent performance, have more
For being widely applied prospect.
In the application process of material, needing material to stand the test of high temperature under increasing operating mode, this is accomplished by material
The coating on material surface has preferable resistance to elevated temperatures, i.e. still can maintain good workability under the operating mode of higher temperature
Can, and be unlikely to significantly to reduce due to the performance appearance that affects of high temperature, and in most cases need coating at high temperature to protect
Hold higher hardness and preferable wearability.For cobalt metal, can undergo phase transition at 400 DEG C, γ phase in version be α phase,
Occurring oxidation to form CoO, wherein α-Co has the structure being similar to graphite, has stacking fault, has kollag simultaneously
Performance, CoO then has more higher hardness than Co, can also play the effect of dry lubrication in friction process simultaneously, permissible
Find out that cobalt has more excellent resistance to elevated temperatures, thus elect the matrix metal of composite deposite as.Cr3C2Granule then has well
High temperature stability performance, hardness is high, and wearability is good, thus the hard phase of composite deposite is done in choosing.
The preparation of high temperature resistant composite deposite needs the key technical problem solved is how to allow Second Phase Particle and matrix metal
Realize codeposition, i.e. should improve the content of composite particles, ensure composite particles being uniformly distributed in coating again.Utilizing
When groove coating technology carries out the preparation of composite deposite, because of hard particles free settling in composite plating bath, and particle arrives cathode surface
Speed relatively slow, quantity delivered is less, limits the deposition of matrix metal and the cladding to hard particles, and coating growth is relatively slow,
Particles dispersed amount is relatively low；Composite plating bath in coating bath is stirred by the mode often through mechanical agitation or ultrasonic wave added, carries
The uniformity of high composite plating bath, simultaneously by liquid being stirred the speed and quantity that in raising plating solution, particle supplies to negative electrode,
Promote the carrying out of codeposition.But meanwhile, the plating solution of agitation can produce certain souring to cathode surface, it is unfavorable for
Being combined of grain, therefore, uses the method for groove plating to be difficulty with granule, and the particularly high-quality of large-size particle is combined.Utilization is penetrated
Stream electrodeposition technology substitutes groove depositing process, and composite plating bath can be delivered directly to cathode surface by it, and the most constantly circulation also makes
Obtain the state that composite plating bath can remain uniform and stable, and this method also can realize selective electrodeposition.Utilize this technology
The compound quantity of granule can be improved to a certain extent, but generally speaking compound quantity is still within reduced levels, meanwhile, this technique
Also there is the shortcomings such as deposited coating and metal structure are loose, deposition velocity is the fastest.Jet electrodeposition process is applied
Ultrasonic technology assists, and can be effectively improved the stability of plating solution and the response speed of electro-deposition, improves coating
Performance, the effect of dispersion solid particle can be played during electrodeposited composite coatings simultaneously, but used at present and surpass
Though sound assisted jet electro-deposition carries out the preparation of composite deposite preferably solves the dispersed problem of solid particle, but fails
Realize being greatly improved the breakthrough of Particles dispersed amount.The pulse power is utilized to replace DC source, in certain journey in electrodeposition process
Coating structure sex chromosome mosaicism produced by jet electro-deposition techniques is solved so that coating more even compact, surfacing on degree
Degree and brightness are all obviously improved, and internal fault of construction significantly reduces, but the compound quantity of granule improves less.Plated by change
Liquid main salt kind and add the method for various additives in plating solution and also can improve coating structure, improves Particles dispersed amount and plating
Layer performance, but it is limited to promote effect.
During preparing composite deposite, both needed both may improve granule content in coating, be also required to simultaneously
Promote the scattered uniformity in coating of granule.Therefore when the main technologic parameters of composite deposite is prepared in consideration then by can shadow
Ring above-mentioned both sides parameter to set about.Granule mass fraction in coating mainly by granule in the quantity delivered of cathode surface and
The impact of the sedimentation rate of the time of staying and matrix metal, the consumption of the main salt of metal, electric current density, pH, the consumption of conducting salt, the moon
The state modulator such as anode relative moving speed deposition and the sedimentation rate of matrix metal, this to can timely and effectively to
The height of the relative amount that grain carries out metal and the granule being coated with and being deposited has material impact；Plating solution flow, granule are used
The parameters such as amount, anode and cathode relative moving speed then in the supply of cathode surface and can stop generation impact on granule, and quantity delivered is more
Less, the time of staying the shortest, then metal is the most difficult to its process being coated with, and granule compound quantity in coating is the lowest.Ultrasound wave has
There is the effect of dispersion agglomerated particle, the dispersibility that granule can be promoted and the uniformity being distributed in coating, but simultaneously also can shadow
Ring the granule stop at cathode surface, it is therefore desirable to carry out selecting control to the parameter of ultrasound wave.
Summary of the invention
The present invention is on the basis of jet electro-deposition techniques, by controlling plating solution flow, anode and cathode relative moving speed two
Individual parameter, it is achieved that micron order Cr during codeposition3C2Effectively being combined of granule, Particles dispersed amount in being obviously improved coating
On the basis of, enhance composite deposite performance.
By the major parameter determined is researched and analysed discovery, composite electrodeposition process is had different by each parameter
, there is respective more excellent parameter area in affecting laws.But during composite electrodeposition, the change of a certain parameter can cause remaining
The more excellent working range of parameter changes therewith, and therefore the present invention can prepare granular mass mark in coating according to different technique
Composite deposite between 9%～31%.
A kind of Co-Cr3C2The preparation technology of high-temperaure coating, is characterized in that: coating is Co-Cr3C2Multiple
Close coating, wherein Cr3C2Particles dispersed quality 9～31%,
The composition of electro-deposition plating solution is: cobalt sulfate 400～500g/L, sodium chloride 15～25g/L, boric acid 20～35g/
L, nickeliferous Cr3C2Granule 350～600g/L, dispersant selects cetyl trimethyl ammonia bromide (CTAB) 0.1～0.5g/L；Institute
State composite deposite hardness and wear resistance after the heating and be not less than room temperature level；Use electro-deposition method, temperature 30～50 DEG C, pH
2～6, electric current density 15～45A/dm2, plating solution flow 1.9～2.4L/min, anode and cathode relative moving speed
1～9mm/s；
Further, nickeliferous Cr3C2Extra-granular cladding layer of metal nickel, the mass fraction of nickel is integral particle quality
20%-50%.
Further, technique for preparing coating is: temperature 30～50 DEG C, pH 2～6, electric current density 15～45A/dm2, plating solution stream
Amount 1.9～2.4L/min, anode and cathode relative moving speed 1～9mm/s, supersonic frequency 20-40KHz, ultrasonic power density 0.1～
3.5W/cm2, the ultrasonic intermittent time 1～8s.
Use the carrying out of the most ultrasonic mode assisted jet electrodeposition process, further increase the compound quantity of granule,
And coating structure is adjusted and improves, coating internal flaw reduces, and structure is finer and close, and performance is the most excellent.
At Cr3C2Granule periphery cladding metallic nickel, improves the combination of matrix metal and hard particles, can remove Composite Coatings from
The vacuum high-temperature of rear coating processes.
Compared with prior art, the present invention is utilized can to realize hard during composite deposite is prepared in jet electro-deposition
The high-quality of grain is combined, and improves the uniformity that granule is distributed in coating, improves composite plating layer structure, and coating is 700
Higher hardness and preferable anti-wear performance still can be maintained under DEG C hot conditions.
Accompanying drawing explanation
Fig. 1 embodiment device schematic diagram
Fig. 2 coating surface morphology and Elemental redistribution
The hardness of coating after the cooling of Fig. 3 different temperatures heat treatment
The coefficient of friction of coating after the cooling of Fig. 4 different temperatures heat treatment
The wear volume of coating after the cooling of Fig. 5 different temperatures heat treatment
Detailed description of the invention
Embodiment 1:
45 steel workpiece surfaces after pretreatment, with jet electro-deposition method at its coating surface Co-Cr3C2Composite deposite.Its
Coating method is:
1) configuration composite plating bath, consisting of: CoSO4·7H2O 430g/L, NaCl 25g/L, H3BO335g/L, CTAB
0.2g/L, pH=3,.Operating procedure is: electric current density 37A/dm2, temperature is 40 DEG C, and plating solution flow is 2.2L/min, anode and cathode
Relative moving speed is 3.0mm/s；
2) 45 steel workpiece surfaces are carried out electric clean, activation processing, and use nickel bottoming as transition zone；
3) sedimentation time is 30min.
Obtained coating is pure cobalt coating, and coating hardness is 374HV, and coating coefficient of friction is 0.786, and wear volume is
5.888×10-3mm3。
Embodiment 2:
1) configuration composite plating bath, consisting of: CoSO4·7H2O 430g/L, NaCl 20g/L, H3BO335g/L, CTAB
0.1g/L, nickeliferous (nickel mass content is nickeliferous Cr3C2The 30%-35% of granule, following example are identical) Cr3C2Granule
350g/L, pH=4.Operating procedure is: electric current density 35A/dm2, temperature is 40 DEG C, and plating solution flow is 2.2L/min, anode and cathode
Relative moving speed is 3mm/s；
2) 45 steel workpiece surfaces are carried out electric clean, activation processing, and use nickel bottoming as transition zone；
3) sedimentation time is 30min.
Obtained composite deposite, Cr3C2The mass fraction of granule is 9.2%, and coating hardness is 485.4HV, coating friction
Coefficient is 0.538, and wear volume is 2.052 × 10-3mm3。
Embodiment 3:
4) configuration composite plating bath, consisting of: CoSO4·7H2O 450g/L, NaCl 20g/L, H3BO330g/L, CTAB
0.3g/L, nickeliferous Cr3C2Granule 500g/L, pH=3.Operating procedure is: electric current density 40A/dm2, temperature is 40 DEG C, plating solution stream
Amount is 2.3L/min, and anode and cathode relative moving speed is 3mm/s；
5) 45 steel workpiece surfaces are carried out electric clean, activation processing, and use nickel bottoming as transition zone；
6) sedimentation time is 30min.
Obtained composite deposite, Cr3C2The mass fraction of granule is 15.4%, and coating hardness is 552HV, coating friction
Coefficient is 0.445, and wear volume is 1.453 × 10-3mm3。
Embodiment 4:
1) configuration composite plating bath, consisting of: CoSO4·7H2O 430g/L, NaCl 25g/L, H3BO335g/L, CTAB
0.2g/L, nickeliferous Cr3C2Granule 450g/L, pH=3.Operating procedure is: electric current density 37A/dm2, temperature is 40 DEG C, plating solution stream
Amount is 2.2L/min, and anode and cathode relative moving speed is 1.2mm/s, and ultrasonic power density is 0.7W/cm2, ultrasound duty cycle is
50%, the intermittent time is 4s, and supersonic frequency is 20kHz；
2) 45 steel workpiece surfaces are carried out electric clean, activation processing, and use nickel bottoming as transition zone；
3) sedimentation time is 30min.
Obtained composite deposite, Cr3C2The mass fraction of granule is 31.4%, and coating hardness is 649HV, coating friction
Coefficient is 0.326, and wear volume is 0.826 × 10-3mm3。
Comparative example 2, example 3 and example 4, by controlling different technological parameters, Cr in prepared composite deposite3C2Granule
Mass fraction is gradually promoted to 15.4% and 31.4% by 9.2%, and the compound quantity of granule can improve more than 3 times, and composite deposite is hard
Degree also by granular mass mark be 485.4HV when 9.2% improve to granular mass mark be 649HV when 31.4%, compound
The 374HV of the hardness purer cobalt coating of coating promotes 29.8% to 73.5%.The coefficient of friction of composite deposite and wear volume are also
Reduce with the increase of granular mass mark in coating.
Example 4 coating is polished, under scanning electron microscope (12000X) to composite deposite in Cr3C2Dividing of granule
Cloth and coated state are analyzed, and shown in the surface topography of composite deposite such as Fig. 2 (a), have obvious second between matrix metal
Phase particulate material, carries out energy spectrum analysis to this material, and the content of its composition result Cr element and Co element is respectively 81% He
8%, thus to infer, particulate material is Cr3C2Granule.
Coating surface is carried out element Surface scan analysis, the distribution situation of the elements such as cobalt, chromium, carbon, nickel respectively as Fig. 2 (b),
2 (c), 2 (d) and 2 (e) are shown, it can be seen that the position of cobalt element is consistent with the matrix location in Fig. 2 (a), the position of chromium element
Putting distribution then consistent with the distribution of Second Phase Particle shape material, the cladding being simultaneously with nickel element outside chromium element exists, and confirms
Cr3C2Granule being combined in cobalt matrix metal, simultaneously by Fig. 2 (a) it can also be seen that coating surface is comparatively dense, internal structure
Middle existence cavity and hole are less, and coating structure is optimised.
Heating the coating of example 1, example 2, example 3 and example 4 in different temperatures, carry out testing hardness after cooling, test load is
100gf, the load time is 15s, and test result is as shown in Figure 3.Pure cobalt coating hardness after heat treatment remains unchanged substantially, compound
The coating the most relatively room temperature hardness of the hardness after high-temperature heat treatment has promoted.
The coating of example 1, example 2, example 3 and example 4 is carried out heat treatment at different temperatures, after cooling, its wearability is surveyed
Examination, test uses CETR-Ш type friction wear testing machine, and friction pair is GCr15 steel ball, and abrasive manner is reciprocating friction, load
For 5N, friction pair speed of related movement is 3mm/s, and reciprocal distance is 4mm, and the testing time is 15min, after abrasion terminates, utilizes
The wear scar width of coating is measured by 3D Laser Measurement microscope, and then calculates wear volume.The test result of coefficient of friction
And the result of calculation of wear volume is as shown in Figure 4 and Figure 5, after high-temperature heat treatment, coefficient of friction and the wear volume of coating all occur
After a certain degree of reduction, i.e. high-temperature heat treatment, cladding wearability increases.
Claims (3)
1. a preparation method for high temperature resistant composite deposite, is characterized in that: Co-Cr3C2Cr in composite deposite3C2Particles dispersed quality
9～31%；
The composition of electro-deposition plating solution is: cobalt sulfate 400～500g/L, sodium chloride 15～25g/L, and boric acid 20～35g/L contains
Nickel Cr3C2Granule 350～600g/L, dispersant selects cetyl trimethyl ammonia bromide 0.1～0.5g/L；Use electro-deposition side
Method, temperature is 30～50 DEG C, pH 2～6, electric current density 15～45A/dm2, plating solution flow 1.9～2.4L/min, anode and cathode phase
It is 1～9mm/s to translational speed.
Preparation method the most according to claim 1, is characterized in that: nickeliferous Cr3C2Extra-granular cladding layer of metal nickel, nickel
The 20%-50% that mass fraction is integral particle quality.
Preparation method the most according to claim 1, is characterized in that: temperature 30～50 DEG C, pH2～6, electric current density 15～
45A/dm2, plating solution flow 1.9～2.4L/min, anode and cathode relative moving speed 1～9mm/s, and supersonic frequency 20-40KHz,
Ultrasonic power density 0.1～3.5W/cm2, the ultrasonic intermittent time 1～8s.
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Cited By (5)
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| CN109267124A (en) * | 2018-10-19 | 2019-01-25 | 西安西电电气研究院有限责任公司 | A kind of silver coated graphite composite deposite and preparation method thereof |
| CN112226805A (en) * | 2020-10-26 | 2021-01-15 | 矿冶科技集团有限公司 | Preparation method of electrodeposited cobalt-based composite coating |
| CN112281201A (en) * | 2020-10-30 | 2021-01-29 | 中冶赛迪技术研究中心有限公司 | Equipment and process for metal flat surface nano composite electroplating |
| CN112301393A (en) * | 2020-10-30 | 2021-02-02 | 中冶赛迪技术研究中心有限公司 | Equipment and process for nano composite electroplating of inner surface of metal pipe fitting |
| CN112410852A (en) * | 2020-10-30 | 2021-02-26 | 中冶赛迪技术研究中心有限公司 | Nano composite electroplating equipment and electroplating process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109267124A (en) * | 2018-10-19 | 2019-01-25 | 西安西电电气研究院有限责任公司 | A kind of silver coated graphite composite deposite and preparation method thereof |
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| CN112281201A (en) * | 2020-10-30 | 2021-01-29 | 中冶赛迪技术研究中心有限公司 | Equipment and process for metal flat surface nano composite electroplating |
| CN112301393A (en) * | 2020-10-30 | 2021-02-02 | 中冶赛迪技术研究中心有限公司 | Equipment and process for nano composite electroplating of inner surface of metal pipe fitting |
| CN112410852A (en) * | 2020-10-30 | 2021-02-26 | 中冶赛迪技术研究中心有限公司 | Nano composite electroplating equipment and electroplating process |
| CN112301393B (en) * | 2020-10-30 | 2021-12-07 | 中冶赛迪技术研究中心有限公司 | Equipment and process for nano composite electroplating of inner surface of metal pipe fitting |
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